CN114656617A - 一种环氧树脂活性稀释剂的制备方法 - Google Patents
一种环氧树脂活性稀释剂的制备方法 Download PDFInfo
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- 239000003085 diluting agent Substances 0.000 title claims abstract description 20
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 20
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000047 product Substances 0.000 claims abstract description 18
- 239000003513 alkali Substances 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012043 crude product Substances 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 5
- 238000011033 desalting Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims abstract description 4
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 238000007670 refining Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- -1 amine salt Chemical class 0.000 claims description 5
- UGAKJPMSFVMKEF-UHFFFAOYSA-N C=1C=CC=CC=1[P](C=1C=CC=CC=1)(Br)C1=CC=CC=C1 Chemical compound C=1C=CC=CC=1[P](C=1C=CC=CC=1)(Br)C1=CC=CC=C1 UGAKJPMSFVMKEF-UHFFFAOYSA-N 0.000 claims description 3
- WYGVRVDZSPABJU-UHFFFAOYSA-N Cl[P](c1ccccc1)(c1ccccc1)c1ccccc1 Chemical compound Cl[P](c1ccccc1)(c1ccccc1)c1ccccc1 WYGVRVDZSPABJU-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 150000003017 phosphorus Chemical class 0.000 claims description 3
- 238000007127 saponification reaction Methods 0.000 claims description 3
- QWBBPBRQALCEIZ-UHFFFAOYSA-N 2,3-dimethylphenol Chemical compound CC1=CC=CC(O)=C1C QWBBPBRQALCEIZ-UHFFFAOYSA-N 0.000 claims description 2
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 claims description 2
- 239000008346 aqueous phase Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/02—Synthesis of the oxirane ring
- C07D301/24—Synthesis of the oxirane ring by splitting off HAL—Y from compounds containing the radical HAL—C—C—OY
- C07D301/26—Y being hydrogen
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/27—Condensation of epihalohydrins or halohydrins with compounds containing active hydrogen atoms
- C07D301/28—Condensation of epihalohydrins or halohydrins with compounds containing active hydrogen atoms by reaction with hydroxyl radicals
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/12—Compounds containing oxirane rings with hydrocarbon radicals, substituted by singly or doubly bound oxygen atoms
- C07D303/18—Compounds containing oxirane rings with hydrocarbon radicals, substituted by singly or doubly bound oxygen atoms by etherified hydroxyl radicals
- C07D303/20—Ethers with hydroxy compounds containing no oxirane rings
- C07D303/22—Ethers with hydroxy compounds containing no oxirane rings with monohydroxy compounds
- C07D303/23—Oxiranylmethyl ethers of compounds having one hydroxy group bound to a six-membered aromatic ring, the oxiranylmethyl radical not being further substituted, i.e.
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Abstract
本申请公开了一种环氧树脂活性稀释剂的制备方法,依次包括如下步骤:S1准备如下物料:混合酚、环氧氯丙烷、催化剂、碱溶液;S2按比例将所述混合酚、环氧氯丙烷、催化剂混合均匀,在特定温度下加热维持一定时间;S3在步骤S2得到的中间体中加入所述碱溶液,在特定温度下加热维持一定时间,步骤S2中的所述混合酚的重量与步骤S3中的所述碱溶液的重量之比为1:0.8~0.95;S4将S3得到的产物中和至中性,水洗脱盐,得到粗产品;S5将S4得到的粗产品升温时通入氮气,在一定真空度下进行真空汽提精制脱水,去除前馏分的水和小分子物,得到产品。本发明工艺稳定可靠,产品稳定,得到的产品技术参数优异。
Description
技术领域
本发明涉及化工领域,特别涉及一种环氧树脂活性稀释剂的制备方法。
背景技术
环氧树脂稀释剂是配合基础树脂混合使用,可以降低固化体系粘度,增加流动性,延长使用寿命,便于大面积施工;改善了操作性的同时,又不影响固化物的基本性能。方便用于浇铸、灌注、粘接、密封、浸渍等方面之应用。
发明内容
本发明的目的在于提供一种环氧树脂活性稀释剂的制备方法。
为实现上述目的,本发明提供如下技术方案。
本申请实施例公开了一种环氧树脂活性稀释剂的制备方法,依次包括如下步骤:
S1准备如下物料:混合酚、环氧氯丙烷、催化剂、碱溶液;
S2按比例将所述混合酚、环氧氯丙烷、催化剂混合均匀,在特定温度下加热维持一定时间,所述环氧氯丙烷的加入量为所述混合酚重量的80~88%,所述催化剂的加入量为所述混合酚重量的0.1~1.0%;
S3在步骤S2得到的中间体中加入所述碱溶液,在特定温度下加热维持一定时间,步骤S2中的所述混合酚的重量与步骤S3中的所述碱溶液的重量之比为1:0.8~0.95;
S4将S3得到的产物中和至中性,水洗脱盐,得到粗产品;
S5将S4得到的粗产品升温时通入氮气,在一定真空度下进行真空汽提精制脱水,去除前馏分的水和小分子物,得到产品。
优选的,在上述环氧树脂活性稀释剂的制备方法中,所述混合酚为苯酚、甲基苯酚或二甲基苯酚,所述碱溶液为质量浓度46-50%的NaOH溶液,所述催化剂为有机磷盐或有机胺盐,包括三苯基磷氯化物或三苯基磷溴化物或烷基苯胺氯化物。
优选的,在上述环氧树脂活性稀释剂的制备方法中,步骤S2中特定温度为40~70℃,时间为3~6h。
优选的,在上述环氧树脂活性稀释剂的制备方法中,步骤S3中特定温度为40~70℃,时间为3~8h。
优选的,在上述环氧树脂活性稀释剂的制备方法中,步骤S4中,所述中性为水相pH值达到7。
优选的,在上述环氧树脂活性稀释剂的制备方法中,步骤S5中,所述一定真空度为-0.09MPa,在温度为50~160℃下进行真空汽提回收。
优选的,在上述环氧树脂活性稀释剂的制备方法中,步骤S5得到的产品外观为无色至浅黄色透明液体,25℃下粘度为10~30mPa.s,环氧值为0.49~0.59eq/100g,易皂化氯≤500ppm,无机氯≤20ppm,水分≤0.1%。
本发明工艺稳定可靠,产品稳定,得到的产品技术参数优异。
具体实施方式
下面将对本发明实施例中的技术方案进行详细的描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例,都属于本发明保护的范围。
本技术方案制备得到了环氧树脂活性稀释剂,方法如下,
S1准备如下物料:混合酚、环氧氯丙烷、催化剂、碱溶液,混合酚为苯酚、甲基苯酚或二甲基苯酚,碱溶液为质量浓度46-50%的NaOH溶液,催化剂为有机磷盐或有机胺盐,包括三苯基磷氯化物或三苯基磷溴化物或烷基苯胺氯化物;
S2按比例将混合酚、环氧氯丙烷、催化剂混合均匀,在40~70℃温度下加热维持3~6h,环氧氯丙烷的加入量为混合酚重量的80~88%,催化剂的加入量为混合酚重量的0.1~1.0%;
S3在步骤S2得到的中间体中加入碱溶液,在40~70℃温度下加热维持3~8h,步骤S2中的混合酚的重量与步骤S3中的碱溶液的重量之比为1:0.8~0.95;
S4将S3得到的产物中和至pH值达到7,水洗脱盐,得到粗产品;
S5将S4得到的粗产品升温时通入氮气,在真空度为-0.09MPa、温度为50~160℃下进行真空汽提精制脱水,去除前馏分的水和小分子物,得到产品
工艺稳定可靠,产品稳定,得到的产品技术参数优异,最后得到的产品外观为无色至浅黄色透明液体,经检测,参数达到如下:25℃下粘度为10~30mPa.s,环氧值为0.49~0.59eq/100g,易皂化氯≤500ppm,无机氯≤20ppm,水分≤0.1%。
本实施方式只是对本专利的示例性说明而并不限定它的保护范围,本领域人员还可以对其进行局部改变,只要没有超出本专利的精神实质,都视为对本专利的等同替换,都在本专利的保护范围之内。
Claims (7)
1.一种环氧树脂活性稀释剂的制备方法,其特征在于,依次包括如下步骤:
S1准备如下物料:混合酚、环氧氯丙烷、催化剂、碱溶液;
S2按比例将所述混合酚、环氧氯丙烷、催化剂混合均匀,在特定温度下加热维持一定时间,所述环氧氯丙烷的加入量为所述混合酚重量的80~88%,所述催化剂的加入量为所述混合酚重量的0.1~1.0%;
S3在步骤S2得到的中间体中加入所述碱溶液,在特定温度下加热维持一定时间,步骤S2中的所述混合酚的重量与步骤S3中的所述碱溶液的重量之比为1:0.8~0.95;
S4将S3得到的产物中和至中性,水洗脱盐,得到粗产品;
S5将S4得到的粗产品升温时通入氮气,在一定真空度下进行真空汽提精制脱水,去除前馏分的水和小分子物,得到产品。
2.根据权利要求1所述的环氧树脂活性稀释剂的制备方法,其特征在于,所述混合酚为苯酚、甲基苯酚或二甲基苯酚,所述碱溶液为质量浓度46-50%的NaOH溶液,所述催化剂为有机磷盐或有机胺盐,包括三苯基磷氯化物或三苯基磷溴化物或烷基苯胺氯化物。
3.根据权利要求1所述的环氧树脂活性稀释剂的制备方法,其特征在于,步骤S2中特定温度为40~70℃,时间为3~6h。
4.根据权利要求1所述的环氧树脂活性稀释剂的制备方法,其特征在于,步骤S3中特定温度为40~70℃,时间为3~8h。
5.根据权利要求1所述的环氧树脂活性稀释剂的制备方法,其特征在于,步骤S4中,所述中性为水相pH值达到7。
6.根据权利要求1所述的环氧树脂活性稀释剂的制备方法,其特征在于,步骤S5中,所述一定真空度为-0.09MPa,在温度为50~160℃下进行真空汽提回收。
7.根据权利要求1所述的环氧树脂活性稀释剂的制备方法,其特征在于,步骤S5得到的产品外观为无色至浅黄色透明液体,25℃下粘度为10~30mPa.s,环氧值为0.49~0.59eq/100g,易皂化氯≤500ppm,无机氯≤20ppm,水分≤0.1%。
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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GB1377246A (en) * | 1971-04-23 | 1974-12-11 | Reichhold Albert Chemie Ag | Process for the manufacture of of glycidyl-ethers |
US4722983A (en) * | 1985-12-13 | 1988-02-02 | Ciba-Geigy Corporation | Process for the preparation of glycidyl compounds |
CN1944487A (zh) * | 2006-09-26 | 2007-04-11 | 蓝星化工新材料股份有限公司无锡树脂厂 | 低有机氯含量的环氧树脂活性稀释剂的制备方法 |
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1377246A (en) * | 1971-04-23 | 1974-12-11 | Reichhold Albert Chemie Ag | Process for the manufacture of of glycidyl-ethers |
US4722983A (en) * | 1985-12-13 | 1988-02-02 | Ciba-Geigy Corporation | Process for the preparation of glycidyl compounds |
CN1944487A (zh) * | 2006-09-26 | 2007-04-11 | 蓝星化工新材料股份有限公司无锡树脂厂 | 低有机氯含量的环氧树脂活性稀释剂的制备方法 |
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