Patent US4136206A successfully refreshed from Google Patents.
US4136206A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method of obtaining a smoking agent
Assignee: Lodz University of Technology
•
Filing: 1977-03-28
•
Granted: 1979-01-23
•
Expires: 1997-03-28
Abstract
Abstract A method for obtaining a smoking agent from smoke condensate obtained from the destructive distillation of cellulose or lignin material comprising subjecting the smoke condensate to extraction by an aqueous solution of a mineral acid to remove organic bases or with a mineral acid which does not decompose at temperatures up to 250° C, in order to bind the bases. The product is then subjected to distillation under reduced pressure in an atmosphere of an inert gas with the addition of metallic dusts and in a second stage of distillation with the addition of a polyhydric alcohol. The obtained smoking agent from the distillation can be subjected to selective absorption of ballast or undesirable substances by passage through suitable adsorbents. In a modification the two stage distillation preceeds the extraction and in a further modification the active substances are first extracted with an organic solvent and then subjected to distillation under reduced pressure.
Inventors
- 👤 Janusz Kulesza
- 👤 Kazimierz Miler
- 👤 Jerzy Podlejski
- 👤 Jozef Gora
- 👤 Teresa Czajkowska
- 👤 Zbigniew Kozlowski
- 👤 Jadwiga Kolska
- 👤 Jolanta Stolowska
- 👤 Zygmunt Rutkowski
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-07 03:16
CPC Classifications
A; A23; A23L; A23L27/00; A23L27/20; A23L27/27
Claims Analysis
Total Claims: 41
Claim 1
Independent Claim
235 words
A method of obtaining a smoking agent from a smoke condensate obtained from the destructive distillation of cellulosic or lignin material comprising extracting the smoke condensate with extracting amounts of aqueous solution of a mineral acid to remove organic nitric bases thereby leaving a purified condensate and then effecting a two-stage distillation of said purified condensate under reduced pressure in an inert gas atmosphere in the presence of anti-oxidative amounts of zinc dust, aluminum dust or iron dust added to said purified condensate, the first stage of the distillation being conducted at a pressure of 20-30 mm Hg to yield a residue and a fraction constituting technological waste containing substances having a boiling point below 100-110° C. at 20-30 mm Hg, the second stage of the distillation being effected on said residue from the first stage of distillation and being conducted at a pressure lower than the first stage and not exceeding 20 mm Hg in the presence of extractive distillation amounts of polyhydric alcohol added to said residue obtained from the first stage, to otain a fraction containing compounds exhibiting a boiling point of up to 250° C. at 20 mm Hg, said fraction from the second stage constituting the smoking agent in admixture with polyhydric alcohol, heating said mixture to a temperature of 50-90° C. to form an alcohol layer and a layer of smoking agent, and separating said layer of smoking agent.
Claim 2
Independent Claim
235 words
A method of obtaining a smoking agent from a smoke condensate obtained from the destructive distillation of cellulosic or lignin material comprising extracting the smoke condensate with extracting amounts of aqueous solution of a mineral acid to remove organic nitric bases thereby leaving a purified condensate and then effecting a two-stage distillation of said purified condensate under reduced pressure in an inert gas atmosphere in the presence of anti-oxidative amounts of zinc dust, aluminum dust or iron dust added to said purified condensate, the first stage of the distillation being conducted at a pressure of 20-30 mm Hg to yield a residue and a fraction constituting technological waste containing substances having a boiling point below 100-110° C. at 20-30 mm Hg, the second stage of the distillation being effected on said residue from the first stage of distillation and being conducted at a pressure lower than the first stage and not exceeding 20 mm Hg in the presence of extractive distillation amounts of polyhydric alcohol added to said residue obtained from the first stage, to otain a fraction containing compounds exhibiting a boiling point of up to 250° C. at 20 mm Hg, said fraction from the second stage constituting the smoking agent in admixture with polyhydric alcohol, heating said mixture to a temperature of 50-90° C. to form an alcohol layer and a layer of smoking agent, and separating said layer of smoking agent.
Claim 3
Dependent Claim
29 words
A method as claimed in claim 1 comprising subjecting said smoking agent to selective adsorption by passing it through an adsorptive mass thereby adsorbing undesirable ballast and noxious compounds.
Claim 4
Dependent Claim
43 words
A method as claimed in claim 1 wherein the extraction of the smoke condensate is effected at room temperature, the aqueous mineral acid solution having a concentration of 5-20% and being present in an amount of 5-25% by weight of the smoke condensate.
Claim 5
Dependent Claim
29 words
A method as claimed in claim 3 comprising subjecting the smoking agent to selective adsorption by passing it through an adsorptive mass thereby adsorbing undesirable ballast and noxious compounds.
Claim 6
Dependent Claim
43 words
A method as claimed in claim 1 comprising neutralizing the fraction, which was obtained from the extraction of the smoke condensate, with water and a member selected from the group consisting of an aqueous solution of sodium bicarbonate and saturated sodium chloride solution.
Claim 7
Dependent Claim
35 words
A method as claimed in claim 5 wherein said mineral acid is orthophosphoric acid in a concentration of 85-90% and is used in a quantity of up to 5% by weight of said smoke condensate.
Claim 8
Dependent Claim
20 words
A method as claimed in claim 1 wherein the inert gas for the distillation is nitrogen, argon or carbon dioxide.
Claim 9
Dependent Claim
37 words
A method as claimed in claim 1 wherein the zinc dust, aluminum dust or iron dust is used in a quantity of 1-10% by weight of said purified condensate obtained by the extraction of the smoke condensate.
Claim 10
Dependent Claim
28 words
A method as claimed in claim 1 wherein the polyhydric alcohol is used in a quantity of 1-10 parts by weight per one part of extracted smoke condensate.
Claim 11
Dependent Claim
13 words
A method as claimed in claim 9 wherein the polyhydric alcohol is glycerol.
Claim 12
Dependent Claim
27 words
A method as claimed in claim 2 wherein the adsorptive mass is selected from the group consisting of active carbon, porous silica gel and synthetic molecular sorbents.
Claim 13
Dependent Claim
54 words
A method as claimed in claim 2 wherein prior to selective adsorption, the smoking agent is diluted with an organic solvent selected from the group comprising: lower aliphatic alcohols, aliphatic ketones, dialkyl ethers and halogenated hydrocarbons, said solvent being used in an amount up to ten times by weight that of said smoking agent.
Claim 14
Dependent Claim
23 words
A method as claimed in claim 2 wherein prior to selective adsorption the smoking agent is heated to a temperature of 50°-90° C.
Claim 15
Independent Claim
184 words
A method of obtaining a smoking agent from a smoke condensate obtained from the destructive distillation of cellulosic or lignin material comprising effecting a two stage distillation of said smoke condensate under reduced pressure in an inert gas atmosphere in the presence of anti-oxidative amounts of zinc dust, aluminum dust or iron dust, said condensate in the first stage of the distillation being subjected to a pressure of 20-30mm Hg to yield a fraction constituting waste exhibiting a boiling point of below 110°-100° C. at a pressure of 20-30 mm Hg and a residue, said residue being subjected in the second stage of the distillation to a pressure lowered to a value that does not exceed 20 mm Hg, to obtain a fraction containing compounds having a boiling point of up to 250° at 20 mm Hg, subjecting the fraction obtained from the second stage of distillation to extraction with an aqueous solution of a mineral acid in amounts to remove organic nitric bases and obtain a remaining tarry fraction, and washing said tarry fraction of mineral acids with water to produce smoking agent.
Claim 16
Independent Claim
184 words
A method of obtaining a smoking agent from a smoke condensate obtained from the destructive distillation of cellulosic or lignin material comprising effecting a two stage distillation of said smoke condensate under reduced pressure in an inert gas atmosphere in the presence of anti-oxidative amounts of zinc dust, aluminum dust or iron dust, said condensate in the first stage of the distillation being subjected to a pressure of 20-30mm Hg to yield a fraction constituting waste exhibiting a boiling point of below 110°-100° C. at a pressure of 20-30 mm Hg and a residue, said residue being subjected in the second stage of the distillation to a pressure lowered to a value that does not exceed 20 mm Hg, to obtain a fraction containing compounds having a boiling point of up to 250° at 20 mm Hg, subjecting the fraction obtained from the second stage of distillation to extraction with an aqueous solution of a mineral acid in amounts to remove organic nitric bases and obtain a remaining tarry fraction, and washing said tarry fraction of mineral acids with water to produce smoking agent.
Claim 17
Dependent Claim
52 words
A method as claimed in claim 14 wherein the extraction of the fraction obtained from the second stage of distillation is carried out at room temperature, the aqueous mineral acid solution having a concentration of 5-20%, and being present in a quantity of 5-25% by weight of the weight of smoke condensate.
Claim 18
Dependent Claim
41 words
A method as claimed in claim 14 wherein the fraction obtained from the extraction of the second stage distillate and washed with water is also washed with neutralizing amounts of aqueous solution of sodium bicarbonate or with saturated sodium chloride solution.
Claim 19
Dependent Claim
14 words
A method as claimed in claim 14 wherein said mineral acid is sulphuric acid.
Claim 20
Dependent Claim
29 words
A method as claimed in claim 14 wherein the zinc dust, aluminum dust or iron dust is used in a quanity of 1-10% by weight of the smoke condensate.
Claim 21
Dependent Claim
29 words
A method as claimed in claim 14 comprising subjecting said smoking agent to selective adsorption by passing it through an adsorptive mass for adsorbing undesirable ballast and noxious compounds.
Claim 22
Dependent Claim
27 words
A method as claimed in claim 19 wherein the adsorptive mass is selected from the group consisting of active carbon, porous silica gel and synthetic molecular sorbents.
Claim 23
Dependent Claim
59 words
A method as claimed in claim 19 wherein prior to selective adsorption the smoking agent is diluted with an organic solvent for said agent selected from the group comprising: lower aliphatic alcohols, aliphatic ketones, dialkyl ethers and halogenated hydrocarbons, said solvent being used in an amount up to ten times greater by weight than the amount of smoking agent.
Claim 24
Dependent Claim
23 words
A method as claimed in claim 19 wherein prior to selective adsorption the smoking agent is heated to a temperature of 50°-90° C.
Claim 25
Independent Claim
141 words
A method of obtaining a smoking agent from tar obtained by condensation of smoke produced from the destructive distillation of cellulosic or lignin material in excess air, comprising subjecting the tar to extraction with an organic solvent to obtain a purified condensate fraction, containing phenols of a molecular weight above 140, subjecting the fraction to distillation under reduced pressure not higher than 20 mm Hg at a temperature of up to 200° C. in the presence of: (a) zinc dust or aluminum dust in amounts to prevent oxidation of quinones and hydroquinones; or (b) non-decomposable mineral acid in amounts to bind organic bases; or (c) a diluent selected from the group consisting of polyhydric alcohols, vegetable oils, high boiling aliphatic hydrocarbons and silicone oils, the distillation process being effected in an oxygen-free atmosphere, and collecting a smoking agent as the distillate.
Claim 26
Independent Claim
141 words
A method of obtaining a smoking agent from tar obtained by condensation of smoke produced from the destructive distillation of cellulosic or lignin material in excess air, comprising subjecting the tar to extraction with an organic solvent to obtain a purified condensate fraction, containing phenols of a molecular weight above 140, subjecting the fraction to distillation under reduced pressure not higher than 20 mm Hg at a temperature of up to 200° C. in the presence of: (a) zinc dust or aluminum dust in amounts to prevent oxidation of quinones and hydroquinones; or (b) non-decomposable mineral acid in amounts to bind organic bases; or (c) a diluent selected from the group consisting of polyhydric alcohols, vegetable oils, high boiling aliphatic hydrocarbons and silicone oils, the distillation process being effected in an oxygen-free atmosphere, and collecting a smoking agent as the distillate.
Claim 27
Dependent Claim
27 words
A method as claimed in claim 23 subjecting the distillate to selective adsorption by passing it through an adsorptive mass to adsorb undesirable ballast and noxious compounds.
Claim 28
Dependent Claim
47 words
A method as claimed in claim 24 wherein the distillation of said condensate fraction is effected in the presence of orthophosphoric acid of a concentration of 85-90% as the mineral acid in a quantity of up to 5% by weight of the fraction subjected to said distillation.
Claim 29
Dependent Claim
35 words
A method as claimed in claim 24 wherein the distillation of said condensate fraction is effected with zinc dust or aluminum dust in a quantity of 1-5% by weight of the fraction subjected to distillation.
Claim 30
Dependent Claim
40 words
A method as claimed in claim 23 wherein the distillation of said condensate fraction is effected with polyhydric alcohol in a quantity of from 3 to 6 parts by weight per 1 part of the fraction subjected to the distillation.
Claim 31
Dependent Claim
13 words
A method as claimed in claim 27 wherein the polyhydric alcohol is glycerol.
Claim 32
Dependent Claim
50 words
A method as claimed in claim 23 wherein the distillation of said condensate fraction is effected in the presence of a diluent selected from the group consisting of polyhydric alcohol and vegetable oils, the distillate being subjected to extraction with extracting amount of a mineral acid, and then to neutralization.
Claim 33
Dependent Claim
27 words
A method as claimed in claim 24 wherein the adsorptive mass is selected from the group consisting of active carbon, porous silica gel and synthetic molecular sorbents.
Claim 34
Dependent Claim
59 words
A method as claimed in claim 24 wherein prior to the selective adsorption process, the distillate is diluted with an organic solvent for the distillate selected from the group comprising: lower aliphatic alcohols, aliphatic ketones, dialkyl ethers and halogenated hydrocarbons, said solvent being used in an amount up to ten times greater by weight than the amount of distillate.
Claim 35
Dependent Claim
25 words
A method as claimed in claim 24 wherein prior to the selective adsorption process the distillate is heated to a temperature of from 50-90° C.
Claim 36
Independent Claim
203 words
A method of obtaining a smoking agent from a smoke condensate obtained from the destructive distillation of cellulosic or lignin material comprising extracting the smoke condensate with orthophosphoric acid to remove organic nitric bases therein in an inert gas atmosphere, thereby leaving a purified condensate and then effecting a two stage distillation of said purified condensate under reduced pressure in an inert gas atmosphere, the first stage of the distillation being conducted at a pressure of 20-30 mm Hg to yield a residue and a fraction constituting technological waste containing substances having a boiling point below 100-110° C. at 20-30 mm Hg, adding anti-oxidative amounts of zinc dust, aluminum dust or iron dust to said residue, the second stage of the distillation being effected on said dust containing residue from the first stage distillation and being conducted at a pressure lower than the first stage and not exceeding 20 mm Hg to obtain a fraction containing compounds exhibiting a boiling point of up to 250° C. at 20 mm Hg, and subjecting said fraction from the second stage of distillation to selective adsorption by passing it through an adsorptive mass to absorb undesirable ballast and noxious compounds and leave a purified smoking agent.
Claim 37
Independent Claim
203 words
A method of obtaining a smoking agent from a smoke condensate obtained from the destructive distillation of cellulosic or lignin material comprising extracting the smoke condensate with orthophosphoric acid to remove organic nitric bases therein in an inert gas atmosphere, thereby leaving a purified condensate and then effecting a two stage distillation of said purified condensate under reduced pressure in an inert gas atmosphere, the first stage of the distillation being conducted at a pressure of 20-30 mm Hg to yield a residue and a fraction constituting technological waste containing substances having a boiling point below 100-110° C. at 20-30 mm Hg, adding anti-oxidative amounts of zinc dust, aluminum dust or iron dust to said residue, the second stage of the distillation being effected on said dust containing residue from the first stage distillation and being conducted at a pressure lower than the first stage and not exceeding 20 mm Hg to obtain a fraction containing compounds exhibiting a boiling point of up to 250° C. at 20 mm Hg, and subjecting said fraction from the second stage of distillation to selective adsorption by passing it through an adsorptive mass to absorb undesirable ballast and noxious compounds and leave a purified smoking agent.
Claim 38
Dependent Claim
29 words
A method as claimed in claim 33 wherein the zinc dust, aluminum dust or iron dust is used in a quantity of 1-10% by weight of the smoke condensate.
Claim 39
Dependent Claim
27 words
A method as claimed in claim 33 wherein the adsorptive mass is selected from the group consisting of active carbon, porous silica gel and synthetic molecular sorbents.
Claim 40
Dependent Claim
59 words
A method as claimed in claim 33 wherein prior to selective adsorption the smoking agent is diluted with an organic solvent for said agent selected from the group comprising: lower aliphatic alcohols, aliphatic ketones, dialkyl ethers and halogenated hydrocarbons, said solvent being used in an amount up to ten times greater by weight than the amount of smoking agent.
Claim 41
Dependent Claim
23 words
A method as claimed in claim 33 wherein prior to selective adsorption the smoking agent is heated to a temperature of 50-90° C.
References Cited (Backward Citations)
US3106473A
Cited
US3152914A
Cited
US3445248A
Cited
USRE27670E
Cited
US3615729A
Cited
US3903267A
Cited
US3875314A
Cited
US3873741A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1982-01-22 | 1982-07-24 | 1983-01-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-01-22 | 1986-07-24 | 1987-01-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-01-22 | 1990-07-24 | 1991-01-23 | $7700.00 | Window Closed / Lapsed |