CN103772693A - Method for preparing lignin polyether polyols - Google Patents
Method for preparing lignin polyether polyols Download PDFInfo
- Publication number
- CN103772693A CN103772693A CN201410032943.2A CN201410032943A CN103772693A CN 103772693 A CN103772693 A CN 103772693A CN 201410032943 A CN201410032943 A CN 201410032943A CN 103772693 A CN103772693 A CN 103772693A
- Authority
- CN
- China
- Prior art keywords
- reactor
- lignin
- parts
- alkali lignin
- polyether polyols
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention relates to a method for preparing lignin polyether polyols. The method comprises the following steps: (1) adding the following raw materials into a reactor in parts by weight: 30-120 parts of alkali lignin, 20-150 parts of water, 0.5-10 parts of cellulase, 0.5-3 parts of sodium hydroxide, 0.1-50 parts of furfuryl alcohol and 1-15 parts of furfural; raising the temperature of the reactor to be 30-65 DEG C, stirring for 2-6 hours, and preparing enzymatic hydrolysis modified alkali lignin; (2) adding the enzymatic hydrolysis modified alkali lignin prepared in the step (1), liquid-state polyhydric alcohols, a bimetallic catalyst, diethylene glycol and glycerol into the reactor in parts by weight, stirring and raising the temperature to be 80-120 DEG C, introducing a small amount of nitrogen into the bottom of the reactor for carrying out bubbling reaction, vacuumizing, adding 0.01-12 parts of epoxypropane into the reactor, reacting in a closed mode for 1-6 hours under normal pressure, and preparing the lignin polyether polyols. The method for preparing the lignin polyether polyols is simple in steps, byproducts can be reasonably and deeply processed by utilizing corn, and the prepared lignin polyether polyols are stable in physical properties, can serve as novel foam materials and are difficult to deform.
Description
Technical field
The present invention relates to a kind of preparation method of lignin polyether polyvalent alcohol.
Background technology
In the time preparing the alcohols materials such as ethylene glycol, propylene glycol, butanols, be mainly prepared from by corn at present, the by product producing in preparation process cannot rationally utilize, the primverose slag that for example produced and corn alcohol slag, no matter be liquid or solid-state, all belonged to industrial waste in the past, cannot utilize, and these waste materials of safe and harmless processing how, be also an industry difficult problem; Therefore be badly in need of a kind of preparation method who utilizes corn deep processing by product to prepare lignin polyether polyvalent alcohol.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of preparation method of lignin polyether polyvalent alcohol, preparation technology is simple, and prepared lignin polyether polyvalent alcohol has good physicals.
The preparation method of lignin polyether polyvalent alcohol of the present invention, comprises the following steps:
1) raw material of following parts by weight is dropped into reactor: alkali lignin 30-120, water 20-150, cellulase 0.5-10, sodium hydroxide 0.5-3, furfuryl alcohol 0.1-50, furfural 1-15; Reactor is warming up to 30-65 ℃, stirs 2-6 hour, make alkali lignin generation enzyme digestion reaction, make enzymolysis modified alkali lignin;
2) will be through step 1) the enzymolysis modified alkali lignin that makes and liquid polyol, bimetallic catalyst, glycol ether, glycerol drop into reactor by following parts by weight: enzymolysis modified alkali lignin 60-130, liquid polyol 40-70, bimetallic catalyst 0-0.003, glycol ether 20-110, glycerol 30-50; Stirring is warming up to 80-120 ℃, passes into a small amount of nitrogen bubble react by reactor bottom, vacuumizes afterwards, and to the propylene oxide that adds 0.01-12 part in reactor, atmospheric closed reaction 1-6 hour, makes lignin polyether polyvalent alcohol.
The preparation method of lignin polyether polyvalent alcohol of the present invention, in step 2) in: described liquid polyol is the liquid by-product by corn processed propylene glycol, ethylene glycol, butanols.
Compared with prior art beneficial effect of the present invention is: preparation method's step of lignin polyether polyvalent alcohol of the present invention is simple, can rationally utilize corn deep processing by product, technique is simple, prepared lignin polyether polyvalent alcohol stable physical property, can be used as novel foam material, not yielding, can realize refuse reclamation, environmental protection.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is described in further detail.Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention.
A preparation method for lignin polyether polyvalent alcohol, comprises the following steps:
1) raw material of following parts by weight is dropped into reactor: alkali lignin 30-120, water 20-150, cellulase 0.5-10, sodium hydroxide 0.5-3, furfuryl alcohol 0.1-50, furfural 1-15; Reactor is warming up to 30-65 ℃, stirs 2-6 hour, make alkali lignin generation enzyme digestion reaction, make enzymolysis modified alkali lignin;
2) will be through step 1) the enzymolysis modified alkali lignin that makes and liquid polyol, bimetallic catalyst, glycol ether, glycerol drop into reactor by following parts by weight: enzymolysis modified alkali lignin 60-130, liquid polyol 40-70, bimetallic catalyst 0-0.003, glycol ether 20-110, glycerol 30-50; Stirring is warming up to 80-120 ℃, passes into a small amount of nitrogen bubble react by reactor bottom, vacuumizes afterwards, and to the propylene oxide that adds 0.01-12 part in reactor, atmospheric closed reaction 1-6 hour, makes lignin polyether polyvalent alcohol.
The preparation method of lignin polyether polyvalent alcohol of the present invention, in step 2) in: described liquid polyol is the liquid by-product by corn processed propylene glycol, ethylene glycol, butanols.
Preparation method's step of lignin polyether polyvalent alcohol of the present invention is simple, can rationally utilize corn deep processing by product, and technique is simple, prepared lignin polyether polyvalent alcohol stable physical property, can be used as novel foam material, not yielding, can realize refuse reclamation, environmental protection.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, do not departing under the prerequisite of the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (2)
1. a preparation method for lignin polyether polyvalent alcohol, is characterized in that, comprises the following steps:
1) raw material of following parts by weight is dropped into reactor: alkali lignin 30-120, water 20-150, cellulase 0.5-10, sodium hydroxide 0.5-3, furfuryl alcohol 0.1-50, furfural 1-15; Reactor is warming up to 30-65 ℃, stirs 2-6 hour, make alkali lignin generation enzyme digestion reaction, make enzymolysis modified alkali lignin;
2) will be through step 1) the enzymolysis modified alkali lignin that makes and liquid polyol, bimetallic catalyst, glycol ether, glycerol drop into reactor by following parts by weight: enzymolysis modified alkali lignin 60-130, liquid polyol 40-70, bimetallic catalyst 0-0.003, glycol ether 20-110, glycerol 30-50; Stirring is warming up to 80-120 ℃, passes into a small amount of nitrogen bubble react by reactor bottom, vacuumizes afterwards, and to the propylene oxide that adds 0.01-12 part in reactor, atmospheric closed reaction 1-6 hour, makes lignin polyether polyvalent alcohol.
2. the preparation method of lignin polyether polyvalent alcohol according to claim 1, is characterized in that, in step 2) in: described liquid polyol is the liquid by-product by corn processed propylene glycol, ethylene glycol, butanols.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410032943.2A CN103772693B (en) | 2014-01-23 | 2014-01-23 | A kind of preparation method of lignin polyether polyhydric alcohol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410032943.2A CN103772693B (en) | 2014-01-23 | 2014-01-23 | A kind of preparation method of lignin polyether polyhydric alcohol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103772693A true CN103772693A (en) | 2014-05-07 |
| CN103772693B CN103772693B (en) | 2016-06-08 |
Family
ID=50565496
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410032943.2A Active CN103772693B (en) | 2014-01-23 | 2014-01-23 | A kind of preparation method of lignin polyether polyhydric alcohol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103772693B (en) |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105504218A (en) * | 2016-02-03 | 2016-04-20 | 广西吉顺能源科技有限公司 | Solar hard foam heat-preservation material |
| CN105504204A (en) * | 2016-02-03 | 2016-04-20 | 广西吉顺能源科技有限公司 | Polyurethane heat preservation material |
| CN105504203A (en) * | 2016-02-03 | 2016-04-20 | 广西吉顺能源科技有限公司 | Polyurethane rigid foam |
| CN105542104A (en) * | 2016-02-03 | 2016-05-04 | 广西吉顺能源科技有限公司 | Polyurethane hard foam thermal-insulation material |
| CN105585687A (en) * | 2016-02-03 | 2016-05-18 | 广西吉顺能源科技有限公司 | Solar thermal-insulation material |
| CN105601869A (en) * | 2016-02-03 | 2016-05-25 | 广西吉顺能源科技有限公司 | Solar rigid polyurethane foam thermal insulation material |
| CN105601868A (en) * | 2016-02-03 | 2016-05-25 | 广西吉顺能源科技有限公司 | Rigid foam polyurethane thermal insulation material |
| CN105669930A (en) * | 2016-02-03 | 2016-06-15 | 广西吉顺能源科技有限公司 | Thermal insulation material |
| CN105693976A (en) * | 2016-02-03 | 2016-06-22 | 广西吉顺能源科技有限公司 | Polyurethane foam thermal insulation material |
| CN105693974A (en) * | 2016-02-03 | 2016-06-22 | 广西吉顺能源科技有限公司 | Solar polyurethane thermal insulation material |
| CN105693973A (en) * | 2016-02-03 | 2016-06-22 | 广西吉顺能源科技有限公司 | Rigid foam thermal insulation material |
| CN105693975A (en) * | 2016-02-03 | 2016-06-22 | 广西吉顺能源科技有限公司 | Rigid polyurethane foam thermal insulation material |
| CN106562119A (en) * | 2016-10-27 | 2017-04-19 | 重庆文洪水产品养殖有限公司 | Degradable multi-stage controlled-release aquatic-product attractant particles and preparation method thereof |
| CN109265672A (en) * | 2018-09-20 | 2019-01-25 | 南京林业大学 | A method of cellulose base polyether polyol is prepared by raw material of alkali cellulose |
| CN110372854A (en) * | 2019-06-10 | 2019-10-25 | 广东奥克化学有限公司 | A kind of lignin-base polyoxyethylene ether of branched structure and preparation method thereof |
| WO2020109460A1 (en) | 2018-11-29 | 2020-06-04 | Fundacion Tecnalia Research & Innovation | Lignin-based polyols |
| CN113105261A (en) * | 2021-05-25 | 2021-07-13 | 单成敏 | Light self preservation temperature wall body |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103097437A (en) * | 2010-06-10 | 2013-05-08 | 阿文德·马立纳什·拉里 | Process for fractionation of biomass |
-
2014
- 2014-01-23 CN CN201410032943.2A patent/CN103772693B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103097437A (en) * | 2010-06-10 | 2013-05-08 | 阿文德·马立纳什·拉里 | Process for fractionation of biomass |
Non-Patent Citations (1)
| Title |
|---|
| 王关斌等: ""玉米芯资源的综合利用"", 《林产化工通讯》, vol. 39, no. 5, 31 December 2005 (2005-12-31), pages 44 - 47 * |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693976A (en) * | 2016-02-03 | 2016-06-22 | 广西吉顺能源科技有限公司 | Polyurethane foam thermal insulation material |
| CN105585687A (en) * | 2016-02-03 | 2016-05-18 | 广西吉顺能源科技有限公司 | Solar thermal-insulation material |
| CN105504218A (en) * | 2016-02-03 | 2016-04-20 | 广西吉顺能源科技有限公司 | Solar hard foam heat-preservation material |
| CN105542104A (en) * | 2016-02-03 | 2016-05-04 | 广西吉顺能源科技有限公司 | Polyurethane hard foam thermal-insulation material |
| CN105693974A (en) * | 2016-02-03 | 2016-06-22 | 广西吉顺能源科技有限公司 | Solar polyurethane thermal insulation material |
| CN105601869A (en) * | 2016-02-03 | 2016-05-25 | 广西吉顺能源科技有限公司 | Solar rigid polyurethane foam thermal insulation material |
| CN105601868A (en) * | 2016-02-03 | 2016-05-25 | 广西吉顺能源科技有限公司 | Rigid foam polyurethane thermal insulation material |
| CN105693973A (en) * | 2016-02-03 | 2016-06-22 | 广西吉顺能源科技有限公司 | Rigid foam thermal insulation material |
| CN105504203A (en) * | 2016-02-03 | 2016-04-20 | 广西吉顺能源科技有限公司 | Polyurethane rigid foam |
| CN105504204A (en) * | 2016-02-03 | 2016-04-20 | 广西吉顺能源科技有限公司 | Polyurethane heat preservation material |
| CN105669930A (en) * | 2016-02-03 | 2016-06-15 | 广西吉顺能源科技有限公司 | Thermal insulation material |
| CN105693975A (en) * | 2016-02-03 | 2016-06-22 | 广西吉顺能源科技有限公司 | Rigid polyurethane foam thermal insulation material |
| CN106562119A (en) * | 2016-10-27 | 2017-04-19 | 重庆文洪水产品养殖有限公司 | Degradable multi-stage controlled-release aquatic-product attractant particles and preparation method thereof |
| CN109265672A (en) * | 2018-09-20 | 2019-01-25 | 南京林业大学 | A method of cellulose base polyether polyol is prepared by raw material of alkali cellulose |
| WO2020109460A1 (en) | 2018-11-29 | 2020-06-04 | Fundacion Tecnalia Research & Innovation | Lignin-based polyols |
| CN110372854A (en) * | 2019-06-10 | 2019-10-25 | 广东奥克化学有限公司 | A kind of lignin-base polyoxyethylene ether of branched structure and preparation method thereof |
| CN113105261A (en) * | 2021-05-25 | 2021-07-13 | 单成敏 | Light self preservation temperature wall body |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103772693B (en) | 2016-06-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103772693A (en) | Method for preparing lignin polyether polyols | |
| CN102633651B (en) | Toluene diamine recovery from tar waste residues discharged during toluene diisocyanate synthesis | |
| CN102002157B (en) | Aromatic polyester modified polyether polyol and preparation method thereof | |
| CN104119518B (en) | The method of biological organic guanidinesalt catalysis method synthesis poly-(succinic acid-butanediol ester-altogether-tetramethylene adipate) | |
| CN107501548B (en) | Preparation method of bio-based non-isocyanate hybrid polyurethane | |
| CN100519497C (en) | Method for extraction separation of dichloropropanol from dichloropropanol hydrochloric water solution | |
| CN102504239A (en) | Catalyst for preparing polycarboxylate water reducing agent macromonomer and preparation method thereof | |
| Formela et al. | Recent advances in development of waste-based polymer materials: A review | |
| MX2012012117A (en) | Polyols suitable for hot molded foam production with high renewable resource content. | |
| CN104693397A (en) | Method for recycling waste polyurethane product | |
| CN110950750A (en) | Method for preparing levulinic acid by hydrolyzing cellulose in molten salt hydrate | |
| KR20180106865A (en) | Method for producing 2,5-furan dicarboxylic acid using an alkali metal-azolide-based catalyst | |
| CN108129650A (en) | A kind of preparation method of polyether polyol | |
| JP2016522296A (en) | Tannin-containing polyol, method for producing and using the same | |
| CN103275349A (en) | Method for recycling polyols from waste polyurethane materials | |
| Liu et al. | Opportunities in Closed-Loop Molecular Recycling of End-of-Life Polyurethane | |
| CN103755936B (en) | A kind of preparation method of biomass phthalic anhydride polyol | |
| Gilbert et al. | The organic chemistry behind the recycling of poly (bisphenol‐A carbonate) for the preparation of chemical precursors: A review | |
| CN102702029A (en) | Preparation process for tetrabutyl urea | |
| CN108117536A (en) | A kind of method of 1,2-PD and carbon dioxide synthesizing acrylic ester | |
| CN103881074B (en) | A kind of preparation method of biomass polyester polyvalent alcohol | |
| CN102174186A (en) | Catalyst for preparing polyalkyl glycol allyl amyl ether and preparation method thereof | |
| CN105885030A (en) | Method for preparing low molecular weight distribution polyether | |
| CN102757557A (en) | Non-isocyan acid water ultraviolet (UV) polyurethane prepared from natural polyhydroxy saccharides and preparation method thereof | |
| JP2012072280A (en) | Polyurethane decomposed matter, polyurethane, and method for forming polyurethane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |