CN103589315B - A kind of ionic liquid Liquefied wood prepares the method for polyurethane coating - Google Patents
A kind of ionic liquid Liquefied wood prepares the method for polyurethane coating Download PDFInfo
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- CN103589315B CN103589315B CN201310561752.0A CN201310561752A CN103589315B CN 103589315 B CN103589315 B CN 103589315B CN 201310561752 A CN201310561752 A CN 201310561752A CN 103589315 B CN103589315 B CN 103589315B
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- ionic liquid
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Abstract
The invention discloses a kind of method that ionic liquid Liquefied wood prepares polyurethane coating, the vitriol oil and amino acid are obtained by reacting ionic liquid in distilled water, at a certain temperature Liquefied wood, obtain the mixture of viscous form containing polyhydroxy substance; With mixture of viscous form and hexamethylene diisocyanate for main raw material, stannous octoate or dibutyl tin laurate are catalyzer, jointly deposit in case, prepare polyurethane coating at other subsidiary material.The present invention is liquefying agent liquefaction renewable resources-timber with green solvent-ionic liquid, replace the common polyvalent alcohol on market to prepare polyurethane coating with liquefied product, the main component changing polyurethane coating inherently derives from the present situation of the Nonrenewable resources such as oil.
Description
Technical field
The invention belongs to polyurethane coating preparation field, be specifically related to a kind of method that ionic liquid Liquefied wood prepares polyurethane coating.
Background technology
Polyurethane coating is the most general coating variety after Synolac.Polyurethane coating has good springiness, low-temperature curable, moisture solidification, can construct many seasons, low temperature, high humidity workability feature.One of main raw material preparing polyurethane coating is polyether glycol at present.Polyether glycol is petrochemicals.
Day by day exhausted petroleum resources have non-renewable, face raw material sources problem while making polyurethane coating cost higher.
Given this, necessaryly a kind of new renewable resources is sought to prepare polyvalent alcohol.This resource can from the reproducible timber of the Nature.Mierocrystalline cellulose, hemicellulose etc., as the major ingredient of timber, are the polymkeric substance of hydroxyl.The liquefied product of timber can as the substitute of polyether glycol, in order to prepare polyurethane coating.
Summary of the invention
A kind of ionic liquid Liquefied wood is the object of the present invention is to provide to prepare the method for polyurethane coating, with green solvent-ionic liquid be liquefying agent liquefaction renewable resources-timber, replace the common polyvalent alcohol on market to prepare polyurethane coating with liquefied product, the main component changing polyurethane coating inherently derives from the present situation of the Nonrenewable resources such as oil.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method that ionic liquid Liquefied wood prepares polyurethane coating comprises the following steps: the preparation of the synthesis of ionic liquid liquefying agent, ionic liquid Liquefied wood and polyurethane coating.
The synthesis of described ionic liquid liquefying agent comprises the following steps:
(1) sulfuric acid and amino acid are reacted 30-150min for 1:1 in molar ratio at 10-100 DEG C, obtain water white amino acid pattern ionic liquid aqueous solution;
(2), after the moisture evaporation in liquid step (1) obtained, obtain head product, after vacuum-drying, obtain ionic liquid liquefying agent.
Described amino acid is the one in L-Ala, L-glutamic acid, leucine, aspartic acid.
Described ionic liquid Liquefied wood comprises the following steps:
(1) be 2-100:1 mix and blend in mass ratio by ionic liquid liquefying agent and timber, obtain the solidliquid mixture of thickness;
(2) by solidliquid mixture isolated by vacuum filtration, and with distilled water repetitive scrubbing filter residue, until filtrate is in neutral;
(3) vacuum drying oven filter residue that step (2) obtains being put into 80-100 DEG C is dried to constant weight; Weigh filter residue, calculate liquefied fraction;
(4) filtrate that step (2) obtains is neutralized to slightly acidic with barium hydroxide solution, moves into underpressure distillation removing moisture wherein in rotatory evaporator after filtering, and obtain Wood liquefied product through vacuum-drying.
Described timber is pine or China fir.
The preparation of described polyurethane coating comprises the following steps:
(1) hydroxy radical content of Wood liquefied product is detected;
(2) in the presence of the solvent, be that 2:1 takes hexamethylene diisocyanate (HDI) and TriMethylolPropane(TMP) hybrid reaction 0.5-4h at 40-100 DEG C by the mol ratio of-NCO and-OH, obtain uniform liquid, i.e. coating composition A;
(3) solvent, filler, Wood liquefied product, catalyzer and additive are at room temperature uniformly mixed 0.5-1h, obtain uniform dope, i.e. coating composition B;
(4) component A and B component are mixed, obtain polyurethane coating.
Described solvent is one or more mixtures in dimethylbenzene, acetone, butylacetate.
Described filler is one or more mixtures in talcum powder, calcium carbonate, kaolin, calcium sulfate, barium sulfate, silicon-dioxide, Calucium Silicate powder.
Described additive is dimethyl silicone oil.
Described catalyzer is stannous octoate or dibutyl tin laurate.
Remarkable advantage of the present invention is: with green solvent---ionic liquid be liquefying agent liquefaction renewable resources---timber, replace the common polyvalent alcohol on market to prepare polyurethane coating with liquefied product, the main component changing polyurethane coating inherently derives from the present situation of the Nonrenewable resources such as oil.
Embodiment
embodiment 1
Prepare polyurethane coating with ionic liquid Liquefied wood with its liquefied product, comprise the following steps:
Step 1: the vitriol oil of a certain amount of 98% is put into reactor with after the distilled water diluting of 10 times of volumes; Take and H
2sO
4above-mentioned reactor put into by L-Ala solid Deng amount of substance, stirring reaction 2h at 50 DEG C.By mixed solution underpressure distillation removing most of moisture, obtain object ion liquid head product.Object ion liquid head product can obtain object ion liquid after vacuum-drying.
Step 2: be that 10:1 mixes by ionic liquid and the mass ratio of pine, stirring reaction 2h at 100 DEG C, obtains the solidliquid mixture of thickness.By solidliquid mixture isolated by vacuum filtration, and with distilled water repetitive scrubbing filter residue, until filtrate is in neutral.Filtrate is neutralized to slightly acidic with baryta water, more after filtration, underpressure distillation and vacuum-drying obtains Wood liquefied product.
Step 3: using the mixing of the butylacetate of the dimethylbenzene of 12mL, the acetone of 4mL and 18mL as solvent, be foundation with NCO:OH=2, the HDI and the TriMethylolPropane(TMP) that take 26.91g put into reactor, and hybrid reaction 2h at 65 DEG C, obtains coating composition A.
Step 4: add 20mL butylacetate, 16.5g talcum powder, 1mL stannous octoate, 4mL dimethyl silicone oil and the Wood liquefied product of 27g in the reactor and be at room temperature uniformly mixed 30min, obtain coating composition B.
Step 5: component A and B component are mixed, will obtain polyurethane coating and carry out film.Record surface drying time and be less than 3 hours, the time of doing solid work is less than 1 day, and hardness of film is greater than H.
embodiment 2
Prepare polyurethane coating with ionic liquid Liquefied wood with its liquefied product, comprise the following steps:
Step 1: the vitriol oil of a certain amount of 98% is put into reactor with after the distilled water diluting of 10 times of volumes; Take and H
2sO
4above-mentioned reactor put into by L-Ala solid Deng amount of substance, stirring reaction 2h at 30 DEG C.By mixed solution underpressure distillation removing most of moisture, obtain object ion liquid head product.Object ion liquid head product can obtain object ion liquid after vacuum-drying.
Step 2: be that 20:1 mixes by ionic liquid and the mass ratio of pine, stirring reaction 2h at 100 DEG C, obtains the solidliquid mixture of thickness.By solidliquid mixture isolated by vacuum filtration, and with distilled water repetitive scrubbing filter residue, until filtrate is in neutral.Filtrate is neutralized to slightly acidic with baryta water, more after filtration, underpressure distillation and vacuum-drying obtains Wood liquefied product.
Step 3: using the mixing of the butylacetate of the dimethylbenzene of 6mL, the acetone of 2mL and 9mL as solvent, be foundation with NCO:OH=2, the HDI and the TriMethylolPropane(TMP) that take 13.5g put into reactor, and hybrid reaction 2h at 65 DEG C, obtains coating composition A.
Step 4: add 24mL butylacetate, 10g talcum powder, 0.5mL stannous octoate, 6mL dimethyl silicone oil and the Wood liquefied product of 13.5g in the reactor and be at room temperature uniformly mixed 30min, obtain coating composition B.
Step 5: component A and B component are mixed, will obtain polyurethane coating and carry out film.Record surface drying time and be less than 3 hours, the time of doing solid work is less than 1 day, and hardness of film is greater than H.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (1)
1. ionic liquid Liquefied wood prepares a method for polyurethane coating, it is characterized in that: comprise the following steps: the preparation of the synthesis of ionic liquid liquefying agent, ionic liquid Liquefied wood and polyurethane coating;
The synthesis of described ionic liquid liquefying agent comprises the following steps:
(1) sulfuric acid and amino acid are reacted 30-150min for 1:1 in molar ratio at 10-100 DEG C, obtain water white amino acid pattern ionic liquid aqueous solution; Described amino acid is the one in L-Ala, L-glutamic acid, leucine, aspartic acid;
(2), after the moisture evaporation in liquid step (1) obtained, obtain head product, after vacuum-drying, obtain ionic liquid liquefying agent;
Described ionic liquid Liquefied wood comprises the following steps:
(1) be 2-100:1 mix and blend in mass ratio by ionic liquid liquefying agent and timber, obtain the solidliquid mixture of thickness; Described timber is pine or China fir;
(2) by solidliquid mixture isolated by vacuum filtration, and with distilled water repetitive scrubbing filter residue, until filtrate is in neutral;
(3) vacuum drying oven filter residue that step (2) obtains being put into 80-100 DEG C is dried to constant weight; Weigh filter residue, calculate liquefied fraction;
(4) filtrate that step (2) obtains is neutralized to slightly acidic with barium hydroxide solution, moves into underpressure distillation removing moisture wherein in rotatory evaporator after filtering, and obtain Wood liquefied product through vacuum-drying;
The preparation of described polyurethane coating comprises the following steps:
(1) hydroxy radical content of Wood liquefied product is detected;
(2) in the presence of the solvent, be that 2:1 takes hexamethylene diisocyanate and TriMethylolPropane(TMP) hybrid reaction 0.5-4h at 40-100 DEG C by the mol ratio of-NCO and-OH, obtain uniform liquid, i.e. coating composition A;
(3) solvent, filler, Wood liquefied product, catalyzer and additive are at room temperature uniformly mixed 0.5-1h, obtain uniform dope, i.e. coating composition B; Described solvent is one or more mixtures in dimethylbenzene, acetone, butylacetate; Described filler is one or more mixtures in talcum powder, calcium carbonate, kaolin, calcium sulfate, barium sulfate, silicon-dioxide, Calucium Silicate powder; Described additive is dimethyl silicone oil; Described catalyzer is stannous octoate or dibutyl tin laurate;
(4) component A and B component are mixed, obtain polyurethane coating.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310561752.0A CN103589315B (en) | 2013-11-13 | 2013-11-13 | A kind of ionic liquid Liquefied wood prepares the method for polyurethane coating |
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| CN201310561752.0A CN103589315B (en) | 2013-11-13 | 2013-11-13 | A kind of ionic liquid Liquefied wood prepares the method for polyurethane coating |
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| CN103589315A CN103589315A (en) | 2014-02-19 |
| CN103589315B true CN103589315B (en) | 2015-11-18 |
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| CN201310561752.0A Expired - Fee Related CN103589315B (en) | 2013-11-13 | 2013-11-13 | A kind of ionic liquid Liquefied wood prepares the method for polyurethane coating |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710895A (en) * | 2015-03-24 | 2015-06-17 | 湖州国信物资有限公司 | Novel phenolic aldehyde epoxy building coating and preparation method thereof |
| CN106047123A (en) * | 2016-07-27 | 2016-10-26 | 上海巨峰化工有限公司 | Ion liquid modified polyurethane coating and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1129241A (en) * | 1994-09-09 | 1996-08-21 | R·E·哈特实验室公司 | Water based, solvent free or low voc, two-component polyurethane coatings |
| DE19613629A1 (en) * | 1995-04-05 | 1996-10-10 | Kansai Paint Co Ltd | Aqueous coating |
| JPH08277377A (en) * | 1995-04-05 | 1996-10-22 | Kansai Paint Co Ltd | Composition for aqueous coating |
| CN102492384A (en) * | 2011-11-28 | 2012-06-13 | 江南大学 | Method of preparing phenolic resin through liquefaction of lignin by using ionic liquid |
-
2013
- 2013-11-13 CN CN201310561752.0A patent/CN103589315B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1129241A (en) * | 1994-09-09 | 1996-08-21 | R·E·哈特实验室公司 | Water based, solvent free or low voc, two-component polyurethane coatings |
| DE19613629A1 (en) * | 1995-04-05 | 1996-10-10 | Kansai Paint Co Ltd | Aqueous coating |
| JPH08277377A (en) * | 1995-04-05 | 1996-10-22 | Kansai Paint Co Ltd | Composition for aqueous coating |
| CN102492384A (en) * | 2011-11-28 | 2012-06-13 | 江南大学 | Method of preparing phenolic resin through liquefaction of lignin by using ionic liquid |
Non-Patent Citations (4)
| Title |
|---|
| 两种咪唑类离子液体对杉木粉的溶解性能;郭立颖等;《化工学报》;20080531;第59卷(第5期);第1300页 * |
| 木材溶液代替聚醚制备聚氨酯涂料的研究;李厚萍;《中国优秀博硕士学位论文全文数据库（硕士）—工程科技Ⅰ辑》;20041215(第4期);第14,25,31,32页 * |
| 植物纤维原料液化新技术;韦冰等;《纤维素科学与技术》;20120630;第2O卷(第2期);第67-70页 * |
| 氨基酸离子液体研究发展;吴阳等;《渤海大学学报（自然科学版）》;20080331;第29卷(第1期);第2页 * |
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Granted publication date: 20151118 Termination date: 20161113 |