CN105061707A - Preparation method for dimethylolpropionic acid modified water-based phenolic resin - Google Patents
Preparation method for dimethylolpropionic acid modified water-based phenolic resin Download PDFInfo
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- CN105061707A CN105061707A CN201510506577.4A CN201510506577A CN105061707A CN 105061707 A CN105061707 A CN 105061707A CN 201510506577 A CN201510506577 A CN 201510506577A CN 105061707 A CN105061707 A CN 105061707A
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Abstract
The invention relates to a preparation method for dimethylolpropionic acid modified water-based phenolic resin. The preparation method comprises the following steps: mixing flax oil and maleic anhydride at ordinary temperature, and rising temperature to be 240-250 DEG C to obtain a first product; mixing tung oil, polyhydric alcohol and potassium hydroxide, and rising temperature to be 240-250 DEG C; cooling the obtained reaction product to be 170-190 DEG C, adding phthalic anhydride, hydroxymethyl cellulose and benzoic acid, flowing back dimethyl benzene, rising temperature to be 170-190 DEG C and preserving heat for 0.5-1.5 h, and then rising temperature to be 200-210 DEG C and preserving heat for 6-8 h to obtain a second product; mixing butyl ether, 2-5 parts by weight of n-butanol, sodium dodecyl benzene sulfonate, tetramethyl orthosilicate and the first product, then adding the second product, and adding an amine neutralizing agent when the temperature is reduced to be 95-105 DEG C, so as to obtain the water-based phenolic resin. The water-based phenolic resin is good in toughness and benzene-free, and the VOC discharge amount is reduced.
Description
Technical field
The present invention relates to chemical technology field, more particularly, relate to a kind of preparation method of dimethylol propionic acid modified water-soluble resol.
Background technology
Dimethylol propionic acid is a kind of multiduty organic raw material, is chainextender in aqueous polyurethane manufacture, urethane can be made again to obtain automatic emulsifying performance, can be made into the self-emulsifying aqueous polyurethane of excellent in stability; Also for the preparation of aqueous emulsion of polyurethane type hide finishes, it is the upgraded product of traditional aqueous emulsion polyacrylic ester hide finishes; Also can be used as the additive improving vibrin, be used as the raw material etc. manufacturing photosensitive resin and liquid crystal.
Resol is generally a kind of resin produced through high temperature polymerization by tung oil, phthalic anhydride, glycerine, tetramethylolmethane, No. 200 solvent oils, be characterized in good weatherability, but VOC quantity discharged is large in production and application process, safety coefficient is not high, inflammable, explosive in use and transportation, belong to hazardous chemical, huge to the pollution of environment, belong to national columns obsolete product.
Summary of the invention
The technical problem to be solved in the present invention is, for the above-mentioned defect of prior art, provides a kind of dimethylol propionic acid modified water-soluble resol.
The technical solution adopted for the present invention to solve the technical problems is:
Construct a kind of preparation method of dimethylol propionic acid modified water-soluble resol, wherein, adopt the raw material of following weight proportion: oleum lini 40-50 part; Cis-butenedioic anhydride 5-10 part; Tung oil 10-20 part; Polyvalent alcohol 10-16 part; Potassium hydroxide 0.005-0.01 part; Phthalic anhydride 5 parts; 5 parts, phenylformic acid; Butyl ether 3-5 part; Propyl carbinol 2-5 part; Walocel MT 20.000PV 2-3 part; Sodium dodecylbenzene sulfonate 1-3 part; Methyl silicate 1-2 part; And adopt following steps:
(1): mixed by the cis-butenedioic anhydride of the oleum lini of 40-50 weight part and 5-10 weight part under normal temperature, be warming up to 240-250 DEG C, insulation 7-9 hour, obtains the first product;
(2): the potassium hydroxide of the polyvalent alcohol of the tung oil of 10-20 weight part, 10-16 weight part and 0.005-0.01 weight part is mixed, is warming up to 240-250 DEG C and is incubated 1-1.5 hour;
(3): reaction product step 2 obtained is cooled to 170-190 DEG C, add the phthalic anhydride of 5 weight parts, the Walocel MT 20.000PV of 2-3 weight part and the phenylformic acid of 5 weight parts, backflow dimethylbenzene is warming up to 170-190 DEG C and is incubated 0.5-1.5 hour, be warming up to 200-210 DEG C again and be incubated 6-8 hour, obtaining the second product;
(4): the Sodium dodecylbenzene sulfonate of the propyl carbinol of the butyl ether of 3-5 weight part, 2-5 weight part, 1-3 part, the methyl silicate of 1-2 part are mixed with the first product, add the second product again, amine neutralizing agent is added when temperature is down to 95-105 DEG C, make mixture ph be 8.5-9, obtain resol resins.
Preparation method of the present invention, wherein, described preparation method comprises step (5) further: in described resol resins, add water carry out latting drown.
Preparation method of the present invention, wherein, the add-on of described amine neutralizing agent is 5-10 weight part.
Preparation method of the present invention, wherein, described amine neutralizing agent is triethylamine or AMP-95.
Preparation method of the present invention, wherein, described polyvalent alcohol is tetramethylolmethane and/or glycerine.
Resol resins good toughness of the present invention, without benzene, the quantity discharged decreasing VOC, in transport and use procedure, safety coefficient is high, it not only reaches the requirement of oleoresin in technical requirements, and be greatly improved in security, the feature of environmental protection and improve, real embodies safety, environmental protection.
Embodiment
In order to make the object of the embodiment of the present invention, technical scheme and advantage clearly, clear, complete description is carried out below in conjunction with the technical scheme in the embodiment of the present invention, obviously, described embodiment is section Example of the present invention, instead of whole embodiment.Based on embodiments of the invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite not paying creative work, all belongs to protection scope of the present invention.
The dimethylol propionic acid modified water-soluble resol of present pre-ferred embodiments, is made up of the raw material of following weight proportion: oleum lini 40-50 part; Cis-butenedioic anhydride 5-10 part; Tung oil 10-20 part; Polyvalent alcohol 10-16 part; Potassium hydroxide 0.005-0.01 part; Phthalic anhydride 5 parts; 5 parts, phenylformic acid; Butyl ether 3-5 part; Propyl carbinol 2-5 part; Walocel MT 20.000PV 2-3 part; Sodium dodecylbenzene sulfonate 1-3 part; Methyl silicate 1-2 part.Described polyvalent alcohol is tetramethylolmethane and/or glycerine.
In a first embodiment, dimethylol propionic acid modified water-soluble resol is made up of the raw material of following weight proportion: oleum lini 50 parts; Cis-butenedioic anhydride 5 parts; Tung oil 10 parts; Polyvalent alcohol 10 parts; 0.005 part, potassium hydroxide; Phthalic anhydride 5 parts; 5 parts, phenylformic acid; Butyl ether 3 parts; Propyl carbinol 2 parts; Walocel MT 20.000PV 5 parts; Sodium dodecylbenzene sulfonate 3 parts; Methyl silicate 1.995 parts.
In a second embodiment, dimethylol propionic acid modified water-soluble resol is made up of the raw material of following weight proportion: oleum lini 40 parts; Cis-butenedioic anhydride 10 parts; Tung oil 20 parts; Polyvalent alcohol 10 parts; 0.01 part, potassium hydroxide; Phthalic anhydride 5 parts; 5 parts, phenylformic acid; Butyl ether 3 parts; Propyl carbinol 2 parts; Walocel MT 20.000PV 2 parts; Sodium dodecylbenzene sulfonate 1 part; Methyl silicate 1.99 parts.
In the third embodiment, dimethylol propionic acid modified water-soluble resol is made up of the raw material of following weight proportion: oleum lini 40 parts; Cis-butenedioic anhydride 8 parts; Tung oil 12 parts; Polyvalent alcohol 16 parts; 0.008 part, potassium hydroxide; Phthalic anhydride 5 parts; 5 parts, phenylformic acid; Butyl ether 5 parts; Propyl carbinol 2.5 parts; Walocel MT 20.000PV 2.5 parts; Sodium dodecylbenzene sulfonate 2 parts; Methyl silicate 1.992 parts.
In the fourth embodiment, dimethylol propionic acid modified water-soluble resol is made up of the raw material of following weight proportion: oleum lini 45 parts; Cis-butenedioic anhydride 7 parts; Tung oil 15 parts; Polyvalent alcohol 10 parts; 0.01 part, potassium hydroxide; Phthalic anhydride 5 parts; 5 parts, phenylformic acid; Butyl ether 3 parts; Propyl carbinol 5 parts; Walocel MT 20.000PV 2 parts; Sodium dodecylbenzene sulfonate 1 part; Methyl silicate 1.99 parts.
Following steps are adopted to make dimethylol propionic acid modified water-soluble resol:
(1): mixed by the cis-butenedioic anhydride of the oleum lini of 40-50 weight part and 5-10 weight part under normal temperature, be warming up to 240-250 DEG C, insulation 7-9 hour, obtains the first product;
(2): the potassium hydroxide of the polyvalent alcohol of the tung oil of 10-20 weight part, 10-16 weight part and 0.005-0.01 weight part is mixed, is warming up to 240-250 DEG C and is incubated 1-1.5 hour;
(3): reaction product step 2 obtained is cooled to 170-190 DEG C, add the phthalic anhydride of 5 weight parts, the Walocel MT 20.000PV of 2-3 weight part and the phenylformic acid of 5 weight parts, backflow dimethylbenzene is warming up to 170-190 DEG C and is incubated 0.5-1.5 hour, be warming up to 200-210 DEG C again and be incubated 6-8 hour, obtaining the second product;
(4): the Sodium dodecylbenzene sulfonate of the propyl carbinol of the butyl ether of 3-5 weight part, 2-5 weight part, 1-3 part, the methyl silicate of 1-2 part are mixed with the first product, add the second product again, amine neutralizing agent is added when temperature is down to 95-105 DEG C, make mixture ph be 8.5-9, obtain resol resins.
Preferably, above-mentioned preparation method comprises step (5) further: in described resol resins, add water carry out latting drown.
Preferably, the add-on of above-mentioned amine neutralizing agent is 5-10 weight part.
Preferably, above-mentioned amine neutralizing agent is triethylamine or AMP-95.
Resol resins good toughness of the present invention, without benzene, the quantity discharged decreasing VOC, in transport and use procedure, safety coefficient is high, it not only reaches the requirement of oleoresin in technical requirements, and be greatly improved in security, the feature of environmental protection and improve, real embodies safety, environmental protection.
Should be understood that, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (5)
1. a preparation method for dimethylol propionic acid modified water-soluble resol, is characterized in that, adopts the raw material of following weight proportion: oleum lini 40-50 part; Cis-butenedioic anhydride 5-10 part; Tung oil 10-20 part; Polyvalent alcohol 10-16 part; Potassium hydroxide 0.005-0.01 part; Phthalic anhydride 5 parts; 5 parts, phenylformic acid; Butyl ether 3-5 part; Propyl carbinol 2-5 part; Walocel MT 20.000PV 2-3 part; Sodium dodecylbenzene sulfonate 1-3 part; Methyl silicate 1-2 part; And adopt following steps:
(1): mixed by the cis-butenedioic anhydride of the oleum lini of 40-50 weight part and 5-10 weight part under normal temperature, be warming up to 240-250 DEG C, insulation 7-9 hour, obtains the first product;
(2): the potassium hydroxide of the polyvalent alcohol of the tung oil of 10-20 weight part, 10-16 weight part and 0.005-0.01 weight part is mixed, is warming up to 240-250 DEG C and is incubated 1-1.5 hour;
(3): reaction product step 2 obtained is cooled to 170-190 DEG C, add the phthalic anhydride of 5 weight parts, the Walocel MT 20.000PV of 2-3 weight part and the phenylformic acid of 5 weight parts, backflow dimethylbenzene is warming up to 170-190 DEG C and is incubated 0.5-1.5 hour, be warming up to 200-210 DEG C again and be incubated 6-8 hour, obtaining the second product;
(4): the Sodium dodecylbenzene sulfonate of the propyl carbinol of the butyl ether of 3-5 weight part, 2-5 weight part, 1-3 part, the methyl silicate of 1-2 part are mixed with the first product, add the second product again, amine neutralizing agent is added when temperature is down to 95-105 DEG C, make mixture ph be 8.5-9, obtain resol resins.
2. preparation method according to claim 1, is characterized in that, described preparation method comprises step (5) further: in described resol resins, add water carry out latting drown.
3. preparation method according to claim 1, is characterized in that, the add-on of described amine neutralizing agent is 5-10 weight part.
4. preparation method according to claim 3, is characterized in that, described amine neutralizing agent is triethylamine or AMP-95.
5. preparation method according to claim 1, is characterized in that, described polyvalent alcohol is tetramethylolmethane and/or glycerine.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602786A (en) * | 2017-09-18 | 2018-01-19 | 成都道立福科技有限公司 | A kind of preparation method of tung oil-modified phenolic resin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104005261A (en) * | 2014-05-12 | 2014-08-27 | 华东理工大学 | Modified waterborne phenolic resin for automobile engine oil filter paper and preparation method thereof |
| CN104629024A (en) * | 2015-03-09 | 2015-05-20 | 徐强 | Dimethylolpropionic acid modified waterborne phenolic resin and preparation method thereof |
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- 2015-08-18 CN CN201510506577.4A patent/CN105061707A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104005261A (en) * | 2014-05-12 | 2014-08-27 | 华东理工大学 | Modified waterborne phenolic resin for automobile engine oil filter paper and preparation method thereof |
| CN104629024A (en) * | 2015-03-09 | 2015-05-20 | 徐强 | Dimethylolpropionic acid modified waterborne phenolic resin and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602786A (en) * | 2017-09-18 | 2018-01-19 | 成都道立福科技有限公司 | A kind of preparation method of tung oil-modified phenolic resin |
| CN107602786B (en) * | 2017-09-18 | 2019-10-29 | 成都道立福科技有限公司 | A kind of preparation method of tung oil-modified phenolic resin |
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Application publication date: 20151118 |