CN101338022B - Method for preparing synthesizing water-solubility insulating resin from vegetable fat - Google Patents
Method for preparing synthesizing water-solubility insulating resin from vegetable fat Download PDFInfo
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- CN101338022B CN101338022B CN 200810041623 CN200810041623A CN101338022B CN 101338022 B CN101338022 B CN 101338022B CN 200810041623 CN200810041623 CN 200810041623 CN 200810041623 A CN200810041623 A CN 200810041623A CN 101338022 B CN101338022 B CN 101338022B
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- TZDTZJJFJJGVDJ-ONEGZZNKSA-N CC(C(CO1)C2C1=O)N(C1)C1=CC2/C=C/C Chemical compound CC(C(CO1)C2C1=O)N(C1)C1=CC2/C=C/C TZDTZJJFJJGVDJ-ONEGZZNKSA-N 0.000 description 1
- UKVSOXGGGOPLAE-UHFFFAOYSA-N CC(C1C(O2)=O)C=CC(C)C1C2=O Chemical compound CC(C1C(O2)=O)C=CC(C)C1C2=O UKVSOXGGGOPLAE-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a preparation method for synthesizing water-soluble insulation resin with vegetable oil, which is characterized in that the method is as follows: the raw materials are weighed by weight portions; vegetable oil, polyol, polycarboxylic acid and ether solvents are added in a vessel to be heated up to 130 DEG C to 160 DEG C to react for 2 to 3 hours under the protection of nitrogen, are added with organic amine under the state of stirring to thermally react for 0.5 to 1 hour; the temperature is reduced to 80 DEG C to 100 DEG C, de-ionized water is added to continue stirring for 1 to 1.5 hours, and a water-soluble resin system is obtained. Then the system is distilled for 1 to 2 hours to remove part of water and solvents and the water-soluble insulation resin with different solid contents is obtained. The preparation method has the advantages of reduction of the dependence on petroleum resources by adopting the vegetable oil to synthesize, simple process, convenient operation, no emission of harmful gases, good insulating property, small shrinkage, good toughness, high mechanical strength and high heat resistant grades which can reach F grade, and is suitable for the insulation treatment of the motors, the coils, etc.
Description
Technical field
The present invention relates to a kind of preparation method with synthesizing water-solubility insulating resin from vegetable fat, synthetic water soluble resin can be widely used in power tool, automobile and motorcycle with on the insulation processing of series excited motor stator, generator stator-rotator and electric apparatus coil, belongs to the electric insulation processing technology field.
Background technology
The conventional oil solubility insulating resin is used for heat cured system to be needed to add a large amount of organic solvents, and most of solvent directly evaporate in the air during curing, thus serious environment pollution and cause the great wasting of resources.The today of growing to even greater heights, building a conservation-minded society in environmental requirement, can not satisfy the needs of society as the insullac of solvent with oil, it will be day by day limited using, and therefore Vegetable oil lipoprotein be carried out the Water-borne modification processing and become main development trend with water as solvent.And the Water-borne modification of resin mainly adopts emulsion process at present, the size of resin dispersion phase particle is larger in the emulsion, be micron order, the out-of-shape of particle and broad particle distribution, causing emulsion is that oyster white is opaque, and easily is subject to the impact of light, heat, soda acid, impurity etc. and causes less stable; Owing to containing a large amount of emulsifying agents in the lacquer liquid, after solidifying color and luster outward appearance and the insulating property of paint film are brought disadvantageous effect in addition, therefore, greatly limited its application in the electric insulation process field.
Summary of the invention
The purpose of this invention is to provide a kind of method with synthesizing water-solubility insulating resin from vegetable fat, technique is simple.The water soluble resin cost of preparation is low, smell is little, good stability; Cooperate with waterborne curing agent, curing speed is fast, package stability is high, the cured article shrinking percentage is little, good toughness, physical strength are high, is suitable as the insulation processing material of high temperature rise, high rotating speed series machine or generator stator-rotator, coil.
For realizing above purpose; technical scheme of the present invention provides a kind of preparation method with synthesizing water-solubility insulating resin from vegetable fat; it is characterized in that; its method is: agitator is being housed; prolong; in the there-necked flask of dropping funnel; being filled with nitrogen speed is 10mL/min; under the nitrogen protection condition; adding weight percent is 20～40% vegetables oil greases; 5～20% polycarboxylic acids; 5～15% polyvalent alcohols; 0～8% ether solvent; under 130 ℃～160 ℃ insulated and stirred conditions, reacted 2～3 hours; drip 1～10% organic amine; add rear continuation reaction 0.5～1 hour; be cooled to 80 ℃～100 ℃; add 30～60% deionized waters; continue to stir the water soluble resin system that namely got in 1～1.5 hour; then distill 1～2h under 100 ℃ of temperature, remove portion water and solvent obtain the water-soluble insulated resin of different solid contents.
Described Vegetable oil lipoprotein is squeezed by plant materials, has the normal temperature flowability or is solid, contains at least one-C=C-C=C-C=C-key and one-COOH in the molecular structure, is oleum lini or tung oil; Be liquid or solid-state under the described polyvalent alcohol normal temperature, contain 2～4-OH in the molecular structure, be one or more mixture of ethylene glycol, propylene glycol, glycerol, glycol ether, triglycol, TriMethylolPropane(TMP); Contain 2～3-COOH in the described polycarboxylic acid molecular structure, be one or more mixture of oxalic acid, propanedioic acid, the third three acid, terephthalic acid, m-phthalic acid; Be liquid under the described organic amine normal temperature, contain 1～2-NH-in the molecular structure, be methylamine, ethamine, propylamine, quadrol, ethylene glycol amine, propylene diamine, trolamine, N, the mixture of one or more of N-dimethylethanolamine; Be liquid under the described ether solvent normal temperature, contain 1-C-O-C-in the molecular structure, be one or more mixture of methyl ether, ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether.
Preparation method with synthesizing water-solubility insulating resin from vegetable fat provided by the present invention adopts chemical process improved plant grease, the water-soluble insulated resin that preparation can be dissolved each other with water.Because not that physical mechanical means by routine make resin and water form emulsion, but the employing chemical process, reaction principle is as shown below:
-COOH+HO-R1-OH→-COO-R1-OH
Start with from the molecular structure of resin, introduce hydrophilic radical and reach the purpose of dissolving each other with water, so resin is uniformly dispersed in water, the solution transparent and stable is high.Do not use monomer polymerization, adopt Vegetable oil lipoprotein to make matrix resin, the residual harmful solvent significantly reduces, so smell is little, and exhaust gas emission reduces.In the water soluble resin building-up process, technique is simple, and water and solvent can recycle, and has saved cost and has improved again service efficiency.Be difficult under the water soluble resin normal temperature of preparation autohemagglutination occurs, be convenient to store and transportation.
Advantage of the present invention is to adopt Vegetable oil lipoprotein synthesizing water-solubility resin, and synthesis technique is simple, easy to operate, and nonhazardous gas is discharged in the building-up process, the water soluble resin of preparing can dissolve each other with water, transparent, the high smell of package stability is little, and organic solvent content is low; Cooperate curing speed fast with waterborne curing agent; Cured article good insulation preformance, shrinking percentage are little, good toughness, physical strength are high, and temperature classification reaches the F level.
Embodiment
Be described in further detail below in conjunction with embodiment 1,2,3 couples of the present invention:
Embodiment 1:
Vegetable oil lipoprotein is selected oleum lini 24.51%, polycarboxylic acid is selected m-phthalic acid 2.96%, and polyvalent alcohol is selected glycol ether 4.90%, ethylene glycol 2.94%, and ether solvent is selected methyl ether 0.49%, ethylene glycol monobutyl ether 1.23%, thanomin 5.15%, deionized water 57.82%.
In the 500m1 there-necked flask of agitator, prolong, dropping funnel is housed; add in proportion oleum lini, m-phthalic acid, glycol ether, ethylene glycol, methyl ether, ethylene glycol monobutyl ether; pass into nitrogen protection, flow is 10mL/min, and the control temperature is at 150 ℃; constantly stirring reaction is after 2.5 hours; drip thanomin, react after 1 hour, be cooled to 90 ℃; add again deionized water, stirred 1 hour.Prolong is changed to water distilling apparatus, is warming up to 100 ℃, under whipped state, distillation 1.5h is cooled to room temperature and namely gets the water-soluble insulated resin, for transparent light yellow, without obvious peculiar smell, can dissolve each other with water.Performance index are as follows:
Table one, embodiment 1 performance index
| 1. outward appearance | Faint yellow transparent thick liquid |
| 2. acid number (in solid part) | 82.6mgKOH/g |
| 3. hydroxyl value (in solid part) | 42.2mgKOH/g |
| 4. water-dilutable | Easily dilution, limpid transparent |
| 5. drying varniss time (130 ± 2 ℃) | ≤3h |
Embodiment 2:
The Vegetable oil lipoprotein resin is selected tung oil 24.39%, polycarboxylic acid is selected Tetra hydro Phthalic anhydride 2.46%, polyvalent alcohol is selected ethylene glycol 5.37%, triglycol 1.95%, ether solvent is selected ether 0.49%, propylene glycol monomethyl ether gram 0.98%, organic amine is selected diethanolamine 1.22%, N, N-dimethylethanolamine 6.10%, deionized water 57.04%.
In the 500ml there-necked flask of agitator, prolong, dropping funnel is housed; add in proportion tung oil, Tetra hydro Phthalic anhydride, ethylene glycol, triglycol, ether, propylene glycol monomethyl ether, pass into nitrogen protection, flow is 10mL/min; the control temperature is at 160 ℃; constantly stirring reaction is 2.5 hours, drips N, the N-dimethylethanolamine; react after 1 hour; be cooled to 90 ℃, add again deionized water, stirred 1 hour.Prolong is changed to water distilling apparatus, is warming up to 100 ℃, under whipped state, distillation 1.5h is cooled to room temperature and namely gets the water-soluble insulated resin, is transparent light tan, without obvious peculiar smell, can dissolve each other with water.
Table two, embodiment 2 performance index
| 1. outward appearance | The transparent thick liquid of reddish-brown |
| 2. acid number (in solid part) | 76.2mgKOH/g |
| 3. hydroxyl value (in solid part) | 40.5mgKOH/g |
| 4. water-dilutable | Easily dilution, limpid transparent |
| 5. drying varniss time (130 ± 2 ℃) | ≤2.5h |
Embodiment 3:
Vegetables oil is selected rosin fat 23.10%, polycarboxylic acid is selected MALEIC ANHYDRIDE 3.47%, polyvalent alcohol is selected ethylene glycol 5.77%, glycol ether 2.31%, organic amine is selected N, N-dimethylethanolamine 5.77%, ether solvent are selected butyl ether 0.69%, propylene glycol monomethyl ether 1.15%, deionized water 57.74%.
In the 500ml there-necked flask of agitator, prolong, dropping funnel is housed; add in proportion rosin fat, MALEIC ANHYDRIDE, ethylene glycol, glycol ether, butyl ether, propylene glycol monomethyl ether, pass into nitrogen protection, flow is 10mL/min; the control temperature is at 150 ℃; constantly stirring reaction is 2.5 hours, drips N, the N-dimethylethanolamine; react after 1 hour; be cooled to 90 ℃, add again deionized water, stirred 1 hour.Prolong is changed to water distilling apparatus, is warming up to 100 ℃, under whipped state, distillation 1.5h is cooled to room temperature and namely gets the water-soluble insulated resin, for transparent slightly yellow, has no irritating odor, and can dissolve each other with water.
Table three, embodiment 3 performance index
| 1. outward appearance | Faint yellow transparent thick liquid |
| 2. acid number (in solid part) | 55.5mgKOH/g |
| 3. hydroxyl value (in solid part) | 60.3mgKOH/g |
| 4. water-dilutable | Easily dilution, limpid transparent |
| 5. drying varniss time (130 ± 2 ℃) | ≤3h |
Claims (4)
1. preparation method with synthesizing water-solubility insulating resin from vegetable fat, it is characterized in that, agitator is being housed, prolong, in the there-necked flask of dropping funnel, being filled with nitrogen speed is 10mL/min, under the nitrogen protection condition, adding weight percent is 20～40% Vegetable oil lipoprotein, 5～20% polycarboxylic acids, 5～15% polyvalent alcohols, 0～8% ether solvent, under 130 ℃～160 ℃ insulated and stirred conditions, reacted 2～3 hours, drip 1～10% organic amine, add rear continuation reaction 0.5～1 hour, be cooled to 80 ℃～100 ℃, add 30～60% deionized waters, continue stirring and namely got the water soluble resin system in 1～1.5 hour, then under 100 ℃ of temperature, distill 1～2h, except anhydrating and solvent, obtain the water-soluble insulated resin of different solid contents;
Described Vegetable oil lipoprotein is squeezed by plant materials, has the normal temperature flowability or is solid, contains at least one-C=C-C=C-C=C-key and one-COOH in the molecular structure, is oleum lini, tung oil.
2. a kind of preparation method with synthesizing water-solubility insulating resin from vegetable fat according to claim 1, it is characterized in that, be liquid or solid-state under the described polyvalent alcohol normal temperature, contain 2～4-OH in the molecular structure, be one or more mixture of ethylene glycol, propylene glycol, glycerol, glycol ether, triglycol, TriMethylolPropane(TMP).
3. a kind of preparation method with synthesizing water-solubility insulating resin from vegetable fat according to claim 1, it is characterized in that, contain 2～3-COOH in the described polycarboxylic acid molecular structure, be one or more mixture of oxalic acid, propanedioic acid, the third three acid, terephthalic acid, m-phthalic acid.
4. a kind of preparation method with synthesizing water-solubility insulating resin from vegetable fat according to claim 1, it is characterized in that, be liquid under the described ether solvent normal temperature, contain 1-C-O-C-in the molecular structure, be one or more mixture of methyl ether, ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102453608B (en) * | 2010-10-26 | 2013-09-04 | 中国石油化工股份有限公司 | Method for reducing oil acid value and obtained oil mixture |
| CN102816498B (en) * | 2012-08-21 | 2014-11-05 | 上海电动工具研究所 | Method for preparing water-solubility insulated paint by using epoxy soybean oil |
| CN105348502B (en) * | 2015-12-10 | 2017-11-10 | 苏州太湖电工新材料股份有限公司 | A kind of water-based insulating paint and preparation method thereof |
Citations (7)
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| US3833411A (en) * | 1971-10-18 | 1974-09-03 | Bell Telephone Labor Inc | Articles coated with alkali-soluble polyester-type resins and method of producing them |
| CN1250460A (en) * | 1997-03-17 | 2000-04-12 | 协和油化株式会社 | Polyester resin composition, cured resin, and coating material |
| CN1473860A (en) * | 2003-06-26 | 2004-02-11 | 郑可省 | Process for producing castor oil modified polyarylester graft copolymer textile size and size |
| CN101050272A (en) * | 2007-05-14 | 2007-10-10 | 江苏长江涂料有限公司 | Anticorrosive bottom lacquer of water-soluble alcohol acid, and preparation method |
| CN101070377A (en) * | 2007-05-14 | 2007-11-14 | 江苏长江涂料有限公司 | Water-soluble alcohol-acid resin solution and water-soluble alcohol-acid amino baking paint and preparing method |
| CN101070376A (en) * | 2007-05-14 | 2007-11-14 | 江苏长江涂料有限公司 | Alcohol-acid type wrinkled resin and preparing method |
| CN101148497A (en) * | 2007-10-22 | 2008-03-26 | 苏州巨峰绝缘材料有限公司 | Air-drying water-soluble alkyd resin and preparation method thereof |
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2008
- 2008-08-12 CN CN 200810041623 patent/CN101338022B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3833411A (en) * | 1971-10-18 | 1974-09-03 | Bell Telephone Labor Inc | Articles coated with alkali-soluble polyester-type resins and method of producing them |
| CN1250460A (en) * | 1997-03-17 | 2000-04-12 | 协和油化株式会社 | Polyester resin composition, cured resin, and coating material |
| CN1473860A (en) * | 2003-06-26 | 2004-02-11 | 郑可省 | Process for producing castor oil modified polyarylester graft copolymer textile size and size |
| CN101050272A (en) * | 2007-05-14 | 2007-10-10 | 江苏长江涂料有限公司 | Anticorrosive bottom lacquer of water-soluble alcohol acid, and preparation method |
| CN101070377A (en) * | 2007-05-14 | 2007-11-14 | 江苏长江涂料有限公司 | Water-soluble alcohol-acid resin solution and water-soluble alcohol-acid amino baking paint and preparing method |
| CN101070376A (en) * | 2007-05-14 | 2007-11-14 | 江苏长江涂料有限公司 | Alcohol-acid type wrinkled resin and preparing method |
| CN101148497A (en) * | 2007-10-22 | 2008-03-26 | 苏州巨峰绝缘材料有限公司 | Air-drying water-soluble alkyd resin and preparation method thereof |
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