WO2015058684A1 - Preparation method for waterborne anti-corrosion resin - Google Patents

Preparation method for waterborne anti-corrosion resin Download PDF

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WO2015058684A1
WO2015058684A1 PCT/CN2014/089108 CN2014089108W WO2015058684A1 WO 2015058684 A1 WO2015058684 A1 WO 2015058684A1 CN 2014089108 W CN2014089108 W CN 2014089108W WO 2015058684 A1 WO2015058684 A1 WO 2015058684A1
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parts
acid
epoxy resin
corrosion
aqueous anti
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PCT/CN2014/089108
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French (fr)
Chinese (zh)
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程建军
秦文
王英
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北京金汇利应用化工制品有限公司
廊坊金汇利工业涂料有限公司
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Publication of WO2015058684A1 publication Critical patent/WO2015058684A1/en

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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
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/58—Epoxy resins
    • C08G18/581—Reaction products of epoxy resins with less than equivalent amounts of compounds containing active hydrogen added before or during the reaction with the isocyanate component
    • 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
    • C08G59/40—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 curing agents used
    • 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
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/0804—Manufacture of polymers containing ionic or ionogenic groups
    • C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
    • 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
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/0804—Manufacture of polymers containing ionic or ionogenic groups
    • C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
    • C08G18/0823—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing carboxylate salt groups or groups forming them
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • 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
    • C08G2150/00—Compositions for coatings
    • C08G2150/90—Compositions for anticorrosive coatings

Definitions

  • the invention relates to a preparation method of an aqueous anti-corrosion resin, belonging to the field of anti-corrosion materials.
  • Waterborne epoxy resin has been widely used due to its low VOC content, low price and good construction performance.
  • the commonly used methods for water-based epoxy resin are mechanical method, reverse conversion method, and self-emulsification method.
  • the water-based epoxy resin prepared by the mechanical method and the reverse conversion method has a large particle size and contains an emulsifier, which affects the anti-corrosion effect.
  • the multi-functional amine curing agent is applied to the protection of the substrate such as cement concrete, and the metal corrosion protection. The field is rarely used.
  • the self-emulsification method is a method in which a hydrophilic substance such as a carboxylic acid group or a sulfonic acid group is introduced into an epoxy resin by a chemical method to form an aqueous solution by salt formation.
  • the waterborne epoxy resin obtained by this method has a smaller particle size, the coating film is more dense, and the corrosion resistance is improved to some extent, but some or all of the hydrophilic substances such as carboxylic acid and sulfonic acid remain in the coating film, and water is encountered. It becomes an ionic form again, which has a negative impact on the water resistance and corrosion resistance of the film.
  • the technical problem to be solved by the present invention is to provide a method for preparing a self-drying or baking type water-based anticorrosive resin, solving the deficiencies in the prior art, obtaining an epoxy resin having a small particle diameter, and improving the density of film formation. At the same time, it also enhances the water and corrosion resistance of the film.
  • an aqueous anti-corrosion resin synthesized by the following components: 40 to 98 parts of epoxy resin, 0.5 to 50 parts of acid substance, 0 to 80 parts of modified substance, 0-60 parts of organic solvent and 0.2-18 parts of organic amine, 0-110 parts of deionized water.
  • the modifying substance is selected from one or more of polycyanates, vinyl monomers, peroxides or organic acids.
  • the epoxy resin is a bisphenol A epoxy resin or a bisphenol F epoxy resin, and has an epoxy equivalent range of 150 to 3,500.
  • the modifying substance includes toluene diisocyanate (TDI), hexamethylene diisocyanate (HDI), isophorone diisocyanate (IPDI) or diphenylmethane diisocyanate (MDI), and an adduct thereof Or trimer, acrylic acid, methacrylic acid, methyl methacrylate, butyl acrylate, hydroxyethyl acrylate, styrene, soybean oleic acid, linoleic acid, dehydrated ricinoleic acid, leaf oleic acid, adipic acid One or several.
  • One or more of the organic solvent ethylene glycol monobutyl ether, propylene glycol methyl ether, propylene glycol methyl ether acetate, butanol or alcohol ester 12, N-methylpyrrolidone, diethylene glycol butyl ether.
  • the acid substance is one or more of hydrochloric acid, sulfuric acid, phosphoric acid, pyrophosphoric acid, polyphosphoric acid, citric acid or tartaric acid.
  • the organic amine is one or more of triethylamine, N,N dimethylethanolamine or triethanolamine.
  • the preparation method of the aqueous anti-corrosion resin as described above includes the following steps:
  • the aqueous anti-corrosion resin is obtained by dropwise addition of 0 to 110 parts of deionized water.
  • reaction temperature in the step (1) ranges from 110 to 135 ° C;
  • the feeding temperature and the reaction temperature in the step (3) are in the range of 110 to 135 ° C;
  • the raw material range is: 45 to 75 parts of epoxy resin, 0.5 to 5 parts of acid substance, 10 to 30 parts of modified substance, 20 to 50 parts of organic solvent and 5 to 10 parts of organic amine, 50 to 100 parts.
  • the raw material range is: 55 to 70 parts of epoxy resin, 1 to 3.5 parts of acid substance, 15 to 26 parts of modified substance, 25 to 40 parts of organic solvent and 5 to 8 parts of organic amine, 70 to 90 parts. Ionic water.
  • the invention has the beneficial effects that the aqueous anti-corrosion resin of the invention is prepared by a self-emulsification method, and at the same time, the hydrophilic group can be deactivated with the metal substrate, and is adsorbed on the metal substrate in an orderly manner, thereby improving the coating.
  • the film is resistant to water and corrosion.
  • Pencil hardness ⁇ 4H Impact resistance (cm) 50 Flexibility First level Adhesion ⁇ 1 level Salt spray resistance ⁇ 1000hr
  • the aqueous anticorrosive resin was composed of the following components: E12 epoxy resin 98 g, soybean oil fatty acid 16 g, propylene glycol methyl ether 60 g, tartaric acid 0.5 g, N,N dimethylethanolamine 0.2 g, and deionized water 73 g.
  • the preparation method of the aqueous anticorrosive resin comprises the following steps:
  • the waterborne anticorrosive resin is composed of the following weight components: E51 epoxy resin 82g, two 70 g of acid, 10 g of urethane monomer diphenylmethane diisocyanate (MDI), 25 g of tartaric acid, and 8 g of N,N dimethylethanolamine.
  • the preparation method of the aqueous anticorrosive resin comprises the following steps:
  • the aqueous anticorrosive resin was composed of the following components: E03 epoxy resin 75 g, ethylene glycol monobutyl ether 40 g, phosphoric acid 3 g, triethylamine 8 g, and deionized water 100 g.
  • the preparation method of the aqueous anticorrosive resin comprises the following steps:
  • the waterborne anticorrosive resin is composed of the following components: E20 epoxy resin 60g, ethylene glycol monobutyl ether 10g, phosphoric acid 32g, styrene 15g, butyl acrylate 10g, benzoyl peroxide 0.5 g of acyl group, 3 g of triethylamine, and 55 g of deionized water.
  • the preparation method of the aqueous anticorrosive resin comprises the following steps:
  • the aqueous anticorrosive resin was composed of the following components: 40 g of E51 epoxy resin, 52 g of coconut oil fatty acid, 25 g of propylene glycol methyl ether, 50 g of phosphoric acid, 5 g of N,N dimethylethanolamine, and 36 g of deionized water.
  • the preparation method of the aqueous anticorrosive resin comprises the following steps:

Abstract

The present invention relates to a preparation method for a waterborne anti-corrosion resin, and comprises the following steps: adding 40 to 98 parts of epoxy resin and 0 to 80 parts of modifier, raising the temperature to 90 °C to 150 °C and stirring for reaction until the acid value is less than 3 mgKOH/g, adding 0 to 60 parts of organic solvent, adding 0.5 to 50 parts of acid substance at the temperature of 90 to 150 °C, stirring in a heat-preservation manner for 2 to 3 hr at the temperature of 90 to 150 °C, decreasing the temperature to 70 to 80 °C, dropwise adding 0.2 to 18 parts of organic amine, stirring and preserving heat for 30 to 50 min, dropwise adding 0 to 110 parts of deionized water for emulsification to obtain the waterborne anti-corrosion resin. The modifier is one or more selected from polyisocyanates, vinyl monomers, hyperoxides, or organic acids. This method can produce an epoxy resin having a small particle size, thereby improving the density of film formation, and also enhancing the water resistance and corrosion resistance of the coating; the method can be applied to air-dried or baking-dried anticorrosive paints.

Description

一种水性防腐蚀树脂的制备方法Preparation method of water-based anti-corrosion resin 技术领域Technical field
本发明涉及一种水性防腐蚀树脂的制备方法，属于防腐蚀材料领域。The invention relates to a preparation method of an aqueous anti-corrosion resin, belonging to the field of anti-corrosion materials.
背景技术Background technique
水性环氧树脂因VOC含量低，价格低廉，施工性能好，已被广泛应用。目前常用的环氧树脂水性化的方法有机械法、相反转法、自乳化法。其中机械法、相反转法制备的水性环氧树脂，粒径较大，且含有乳化剂，影响了其防腐蚀效果，多配合胺类固化剂应用于水泥混凝土等基材保护，在金属防腐蚀领域很少使用。自乳化法是通过化学方法在环氧树脂中，引入羧酸基，磺酸基等亲水物质通过成盐的方式实现水性化。这种方法得到的水性环氧树脂粒径较小，涂膜更致密，耐腐蚀性能得到了一定的提高，但羧酸、磺酸等亲水物质部分或全部残留在涂膜，遇到水会再度变为离子形式，对涂膜的耐水，耐腐蚀性能造成了负面影响。Waterborne epoxy resin has been widely used due to its low VOC content, low price and good construction performance. At present, the commonly used methods for water-based epoxy resin are mechanical method, reverse conversion method, and self-emulsification method. Among them, the water-based epoxy resin prepared by the mechanical method and the reverse conversion method has a large particle size and contains an emulsifier, which affects the anti-corrosion effect. The multi-functional amine curing agent is applied to the protection of the substrate such as cement concrete, and the metal corrosion protection. The field is rarely used. The self-emulsification method is a method in which a hydrophilic substance such as a carboxylic acid group or a sulfonic acid group is introduced into an epoxy resin by a chemical method to form an aqueous solution by salt formation. The waterborne epoxy resin obtained by this method has a smaller particle size, the coating film is more dense, and the corrosion resistance is improved to some extent, but some or all of the hydrophilic substances such as carboxylic acid and sulfonic acid remain in the coating film, and water is encountered. It becomes an ionic form again, which has a negative impact on the water resistance and corrosion resistance of the film.
发明内容Summary of the invention
本发明所要解决的技术问题是提供一种自干或烘烤型水性防腐树脂的制备方法，解决现有技术中的不足，得到粒径较小的环氧树脂，提高了成膜的致密程度，同时也增强了涂膜耐水及耐腐蚀性能。The technical problem to be solved by the present invention is to provide a method for preparing a self-drying or baking type water-based anticorrosive resin, solving the deficiencies in the prior art, obtaining an epoxy resin having a small particle diameter, and improving the density of film formation. At the same time, it also enhances the water and corrosion resistance of the film.
本发明达到以上技术效果的技术方案如下：一种水性防腐蚀树脂，由以下组分合成：40～98份环氧树脂，0.5～50份酸类物质，0～ 80份改性物质，0～60份有机溶剂和0.2～18份有机胺，0～110份去离子水。所述改性物质选自多氰酸酯类，乙烯基类单体、过氧化物或者有机酸中的一种或几种。The technical scheme for achieving the above technical effects of the present invention is as follows: an aqueous anti-corrosion resin synthesized by the following components: 40 to 98 parts of epoxy resin, 0.5 to 50 parts of acid substance, 0 to 80 parts of modified substance, 0-60 parts of organic solvent and 0.2-18 parts of organic amine, 0-110 parts of deionized water. The modifying substance is selected from one or more of polycyanates, vinyl monomers, peroxides or organic acids.
所述环氧树脂为双酚A类环氧树脂或双酚F类环氧树脂，其环氧当量范围为150～3500。The epoxy resin is a bisphenol A epoxy resin or a bisphenol F epoxy resin, and has an epoxy equivalent range of 150 to 3,500.
进一步，所述改性物质包括甲苯二异氰酸酯(TDI)、六亚甲基二异氰酸酯(HDI)、异佛尔酮二异氰酸酯(IPDI)或二苯基甲烷二异氰酸酯(MDI)，以及其加成物或三聚体，丙烯酸，甲基丙烯酸，甲基丙烯酸甲酯，丙烯酸丁酯，丙烯酸羟乙酯、苯乙烯、大豆油酸、亚麻油酸，脱水蓖麻油酸、叶子油酸、己二酸中的一种或几种。Further, the modifying substance includes toluene diisocyanate (TDI), hexamethylene diisocyanate (HDI), isophorone diisocyanate (IPDI) or diphenylmethane diisocyanate (MDI), and an adduct thereof Or trimer, acrylic acid, methacrylic acid, methyl methacrylate, butyl acrylate, hydroxyethyl acrylate, styrene, soybean oleic acid, linoleic acid, dehydrated ricinoleic acid, leaf oleic acid, adipic acid One or several.
所述有机溶剂乙二醇单丁醚、丙二醇甲醚、丙二醇甲醚醋酸酯、丁醇或醇酯十二、N-甲基吡咯烷酮，二乙二醇丁醚中的一种或几种。One or more of the organic solvent ethylene glycol monobutyl ether, propylene glycol methyl ether, propylene glycol methyl ether acetate, butanol or alcohol ester 12, N-methylpyrrolidone, diethylene glycol butyl ether.
所述酸类物质为盐酸、硫酸、磷酸、焦磷酸、多聚磷酸、柠檬酸或酒石酸中的一种或几种。The acid substance is one or more of hydrochloric acid, sulfuric acid, phosphoric acid, pyrophosphoric acid, polyphosphoric acid, citric acid or tartaric acid.
所述有机胺为三乙胺、N,N二甲基乙醇胺或三乙醇胺中的一种或几种。The organic amine is one or more of triethylamine, N,N dimethylethanolamine or triethanolamine.
如上所述水性防腐蚀树脂的制备方法，包括以下步骤：The preparation method of the aqueous anti-corrosion resin as described above includes the following steps:
(1)加入40～98份环氧树脂，0～80份改性物质，升温至90℃～150℃下搅拌反应至酸值小于3mgKOH/g；(1) adding 40 to 98 parts of epoxy resin, 0 to 80 parts of the modified substance, and heating to 90 ° C to 150 ° C to stir the reaction to an acid value of less than 3 mg KOH / g;
(2)添加0～60份有机溶剂，(2) adding 0 to 60 parts of organic solvent,
(3)在90～150℃加入0.5～50份酸类物质，在90～150℃下保温搅拌2～3hr；(3) adding 0.5 to 50 parts of acid substance at 90 to 150 ° C, and stirring at 90 to 150 ° C for 2 to 3 hr;
(4)降温至70～80℃，滴加0.2～18份的有机胺，搅拌保温30～50min； (4) cooling to 70 ~ 80 ° C, adding 0.2 ~ 18 parts of organic amine, stirring and holding for 30 ~ 50min;
(5)滴加去离子水0～110份乳化即得到所述水性防腐蚀树脂。(5) The aqueous anti-corrosion resin is obtained by dropwise addition of 0 to 110 parts of deionized water.
进一步，所述步骤(1)中反应温度的范围为110～135℃；Further, the reaction temperature in the step (1) ranges from 110 to 135 ° C;
进一步，所述步骤(3)中加料温度和反应温度的范围为110～135℃；Further, the feeding temperature and the reaction temperature in the step (3) are in the range of 110 to 135 ° C;
进一步，其原料范围为：45～75份环氧树脂，0.5～5份酸类物质，10～30份改性物质，20～50份有机溶剂和5～10份有机胺，50～100份去离子水；Further, the raw material range is: 45 to 75 parts of epoxy resin, 0.5 to 5 parts of acid substance, 10 to 30 parts of modified substance, 20 to 50 parts of organic solvent and 5 to 10 parts of organic amine, 50 to 100 parts. Ionic water
进一步，其原料范围为：55～70份环氧树脂，1～3.5份酸类物质，15～26份改性物质，25～40份有机溶剂和5～8份有机胺，70～90份去离子水。Further, the raw material range is: 55 to 70 parts of epoxy resin, 1 to 3.5 parts of acid substance, 15 to 26 parts of modified substance, 25 to 40 parts of organic solvent and 5 to 8 parts of organic amine, 70 to 90 parts. Ionic water.
本发明的有益效果是：本发明的水性防腐蚀树脂采用自乳化方法制得，同时其亲水性基团可以与金属基材发生钝化，有序的吸附在金属基材上，提高了涂膜的耐水、耐腐蚀性能。The invention has the beneficial effects that the aqueous anti-corrosion resin of the invention is prepared by a self-emulsification method, and at the same time, the hydrophilic group can be deactivated with the metal substrate, and is adsorbed on the metal substrate in an orderly manner, thereby improving the coating. The film is resistant to water and corrosion.
具体实施方式detailed description
以下对本发明的原理和特征进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。The principles and features of the present invention are described below, and the examples are intended to be illustrative only and not to limit the scope of the invention.
本发明水性防腐树脂基本性能见表1。The basic properties of the aqueous anticorrosive resin of the present invention are shown in Table 1.
表1Table 1
检测指标：Detection Indicator: 数据：data:
乳液粒径：Emulsion particle size: ≤10um≤10um
PH:PH: 7～97~9
50℃热储:50 ° C heat storage: ＞100天>100 days
运用本发明水性防腐树脂制备出的涂料基本性能见表2。 The basic properties of the coating prepared by using the aqueous anticorrosive resin of the present invention are shown in Table 2.
表2Table 2
检测指标Detection Indicator 性能performance
铅笔硬度Pencil hardness ≥4H≥4H
耐冲击(厘米)Impact resistance (cm) 5050
柔韧性Flexibility 一级First level
附着力Adhesion ≤1级≤1 level
耐盐雾Salt spray resistance ≥1000hr≥1000hr
实施例1Example 1
水性防腐树脂由以下重量的组分组成：E12环氧树脂98g、大豆油脂肪酸16g、丙二醇甲醚60g、酒石酸0.5g、N,N二甲基乙醇胺0.2g、去离子水73g。The aqueous anticorrosive resin was composed of the following components: E12 epoxy resin 98 g, soybean oil fatty acid 16 g, propylene glycol methyl ether 60 g, tartaric acid 0.5 g, N,N dimethylethanolamine 0.2 g, and deionized water 73 g.
水性防腐树脂的制备方法包括以下步骤：The preparation method of the aqueous anticorrosive resin comprises the following steps:
(1)向装有搅拌器加热套的三口瓶中加入98gE12环氧树脂和16g大豆油脂肪酸；升温至140℃在搅拌的状态下反应至酸值≤3mgKOH/g；(1) adding 98g of E12 epoxy resin and 16g of soybean oil fatty acid to a three-necked flask equipped with a stirrer heating jacket; heating to 140 ° C and reacting to an acid value of ≤ 3mgKOH / g;
(2)加入60g丙二醇甲醚，降温至80℃；(2) adding 60 g of propylene glycol methyl ether, cooling to 80 ° C;
(3)加入0.5g酒石酸，升温至120℃保温3小时；(3) adding 0.5 g of tartaric acid, and heating to 120 ° C for 3 hours;
(4)降温至75℃，滴加0.2gN,N二甲基乙醇胺，在不停的搅拌下，保温30min；(4) cooling to 75 ° C, dropwise addition of 0.2g N, N dimethylethanolamine, with constant stirring, heat for 30min;
(5)在70～80℃缓慢的加入73g去离子水即得到固体含量为50％的水性防腐树脂。(5) 73 g of deionized water was slowly added at 70 to 80 ° C to obtain an aqueous anticorrosive resin having a solid content of 50%.
实施例2Example 2
水性防腐树脂由以下重量的组分组成：E51环氧树脂82g、己二 酸70g、聚氨酯单体二苯基甲烷二异氰酸酯(MDI)10g、酒石酸25g、N,N二甲基乙醇胺8g。The waterborne anticorrosive resin is composed of the following weight components: E51 epoxy resin 82g, two 70 g of acid, 10 g of urethane monomer diphenylmethane diisocyanate (MDI), 25 g of tartaric acid, and 8 g of N,N dimethylethanolamine.
水性防腐树脂的制备方法包括以下步骤：The preparation method of the aqueous anticorrosive resin comprises the following steps:
(1)向装有搅拌器加热套的三口瓶中加入82gE51环氧树脂和70g己二酸，升温至140℃在搅拌的状态下反应至酸值≤3mgKOH/g；(1) adding 82g of E51 epoxy resin and 70g of adipic acid to a three-necked flask equipped with a stirrer heating jacket, and heating to 140 ° C to react to an acid value of ≤ 3mgKOH / g;
(2)降温至110℃，滴加10g二苯基甲烷二异氰酸酯(MDI)单体，40min滴加完毕，95～100℃保温2hr；(2) cooling to 110 ° C, adding 10 g of diphenylmethane diisocyanate (MDI) monomer, 40 minutes after the completion of the addition, 95 ~ 100 ° C for 2 hr;
(3)加入150g乙二醇单丁醚，降温至80℃；(3) adding 150 g of ethylene glycol monobutyl ether, cooling to 80 ° C;
(4)加入25g酒石酸，升温至120℃保温3hr；(4) adding 25g of tartaric acid, heating to 120 ° C for 3 hr;
(5)降温至75℃，滴加8gN,N二甲基乙醇胺，在不停的搅拌下，保温30分钟即得到水性防腐蚀树脂。(5) The temperature was lowered to 75 ° C, 8 g of N, N dimethylethanolamine was added dropwise, and the water-based anticorrosive resin was obtained by keeping it under stirring for 30 minutes.
实施例3Example 3
水性防腐树脂由以下重量的组分组成：E03环氧树脂75g、乙二醇单丁醚40g、磷酸3g、三乙胺8g、去离子水100g。The aqueous anticorrosive resin was composed of the following components: E03 epoxy resin 75 g, ethylene glycol monobutyl ether 40 g, phosphoric acid 3 g, triethylamine 8 g, and deionized water 100 g.
水性防腐树脂的制备方法包括以下步骤：The preparation method of the aqueous anticorrosive resin comprises the following steps:
(1)向装有搅拌器加热套的三口瓶中加入75gE03环氧树脂和40g乙二醇单丁醚升温至140℃，保温30min；(1) adding 75g of E03 epoxy resin and 40g of ethylene glycol monobutyl ether to a three-necked flask equipped with a stirrer heating jacket to raise the temperature to 140 ° C, and keep warm for 30 min;
(2)升温至150℃，滴加入3g磷酸,150℃保温2hr；(2) The temperature is raised to 150 ° C, 3 g of phosphoric acid is added dropwise, and the temperature is kept at 150 ° C for 2 hr;
(3)降温至90℃加入8g三乙胺，搅拌30min；(3) cooling to 90 ° C, adding 8 g of triethylamine, stirring for 30 min;
(4)滴加100g去离子水乳化得到水性防腐蚀环氧树脂。(4) Emulsifying 100 g of deionized water to obtain an aqueous anticorrosive epoxy resin.
实施例4Example 4
水性防腐树脂由以下重量的组分组成：E20环氧树脂60g、乙二醇单丁醚10g、磷酸32g、苯乙烯15g、丙烯酸丁酯10g、过氧化苯甲 酰0.5g、三乙胺3g、去离子水55g。The waterborne anticorrosive resin is composed of the following components: E20 epoxy resin 60g, ethylene glycol monobutyl ether 10g, phosphoric acid 32g, styrene 15g, butyl acrylate 10g, benzoyl peroxide 0.5 g of acyl group, 3 g of triethylamine, and 55 g of deionized water.
水性防腐树脂的制备方法包括以下步骤：The preparation method of the aqueous anticorrosive resin comprises the following steps:
(1)向装有搅拌器加热套的三口瓶中加入60gE20环氧树脂和10g乙二醇单丁醚升温至110℃保温；(1) adding 60 g of E20 epoxy resin and 10 g of ethylene glycol monobutyl ether to a three-necked flask equipped with a stirrer heating jacket to raise the temperature to 110 ° C;
(2)将15g苯乙烯，10g丙烯酸丁酯，0.5g过氧化苯甲酰混合均匀，缓慢均匀的滴加到三口瓶中，2hr滴加完毕。滴加完毕后110℃保温2hr。(2) 15 g of styrene, 10 g of butyl acrylate, and 0.5 g of benzoyl peroxide were uniformly mixed, and slowly and uniformly dropped into a three-necked bottle, and the addition was completed in 2 hours. After the addition was completed, the temperature was kept at 110 ° C for 2 hr.
(3)升温至150℃，滴加入32g磷酸,150℃保温2hr；(3) The temperature is raised to 150 ° C, 32 g of phosphoric acid is added dropwise, and the temperature is kept at 150 ° C for 2 hr;
(4)降温至90℃加入3g三乙胺，搅拌30min。(4) Cooling to 90 ° C, adding 3 g of triethylamine, stirring for 30 min.
(5)加55g去离子水乳化得到防腐蚀树脂乳液。(5) Emulsified with 55 g of deionized water to obtain an anticorrosive resin emulsion.
实施例5Example 5
水性防腐树脂由以下重量的组分组成：E51环氧树脂40g、椰子油脂肪酸52g、丙二醇甲醚25g、磷酸50g、N,N二甲基乙醇胺5g、去离子水36g。The aqueous anticorrosive resin was composed of the following components: 40 g of E51 epoxy resin, 52 g of coconut oil fatty acid, 25 g of propylene glycol methyl ether, 50 g of phosphoric acid, 5 g of N,N dimethylethanolamine, and 36 g of deionized water.
水性防腐树脂的制备方法包括以下步骤：The preparation method of the aqueous anticorrosive resin comprises the following steps:
(1)向装有搅拌器加热套的三口瓶中加入40gE51环氧树脂和52g椰子油脂肪酸，升温至140℃在搅拌的状态下反应至酸值≤3mgKOH/g；(1) adding 40g of E51 epoxy resin and 52g of coconut oil fatty acid to a three-necked flask equipped with a stirrer heating jacket, and heating to 140 ° C to react to an acid value of ≤ 3mgKOH / g;
(2)加入25g丙二醇甲醚，降温至80℃；(2) adding 25 g of propylene glycol methyl ether, cooling to 80 ° C;
(3)加入50g磷酸，升温至120℃保温3hr；(3) adding 50g of phosphoric acid, heating to 120 ° C for 3 hr;
(4)降温至75℃，滴加5gN,N二甲基乙醇胺，在不停的搅拌下，保温30min；(4) Cooling to 75 ° C, adding 5 g of N, N dimethylethanolamine, with constant stirring for 30 min;
(5)在70～80℃缓慢的滴加36g去离子水即得到水性防腐树脂。 (5) 36 g of deionized water was slowly added dropwise at 70 to 80 ° C to obtain an aqueous anticorrosive resin.
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。 The above are only the preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalents, improvements, etc., which are within the spirit and scope of the present invention, should be included in the protection of the present invention. Within the scope.

Claims (10)

  1. 一种水性防腐蚀树脂的制备方法，其特征在于，包括以下步骤：A method for preparing an aqueous anti-corrosion resin, comprising the steps of:
    (1)加入40～98份环氧树脂，0～80份改性物质，升温至90℃～150℃下搅拌反应至酸值小于3mgKOH/g；(1) adding 40 to 98 parts of epoxy resin, 0 to 80 parts of the modified substance, and heating to 90 ° C to 150 ° C to stir the reaction to an acid value of less than 3 mg KOH / g;
    (2)添加0～60份有机溶剂；(2) adding 0 to 60 parts of an organic solvent;
    (3)在90～150℃加入0.5～50份酸类物质，在90～150℃下保温搅拌2～3hr；(3) adding 0.5 to 50 parts of acid substance at 90 to 150 ° C, and stirring at 90 to 150 ° C for 2 to 3 hr;
    (4)降温至70～80℃，滴加0.2～18份的有机胺，搅拌保温30～50min；(4) cooling to 70 ~ 80 ° C, adding 0.2 ~ 18 parts of organic amine, stirring and holding for 30 ~ 50min;
    (5)滴加去离子水0～110份乳化即得到所述水性防腐蚀树脂。(5) The aqueous anti-corrosion resin is obtained by dropwise addition of 0 to 110 parts of deionized water.
  2. 如权利要求1所述之水性防腐蚀树脂的制备方法，其特征在于：所述步骤(1)中反应温度的范围为110～135℃。The method for producing an aqueous anti-corrosion resin according to claim 1, wherein the reaction temperature in the step (1) ranges from 110 to 135 °C.
  3. 如权利要求1所述之水性防腐蚀树脂的制备方法，其特征在于：所述步骤(3)中加料温度和反应温度的范围为110～135℃。The method for producing an aqueous anti-corrosion resin according to claim 1, wherein the feed temperature and the reaction temperature in the step (3) are in the range of 110 to 135 °C.
  4. 如权利要求1所述之水性防腐蚀树脂的制备方法，其特征在于，其原料范围为：45～75份环氧树脂，0.5～5份酸类物质，10～30份改性物质，20～50份有机溶剂和5～10份有机胺，50～100份去离子水。The method for preparing an aqueous anti-corrosion resin according to claim 1, wherein the raw material range is: 45 to 75 parts of an epoxy resin, 0.5 to 5 parts of an acid substance, 10 to 30 parts of a modified substance, 20 to 50 parts of organic solvent and 5-10 parts of organic amine, 50-100 parts of deionized water.
  5. 如权利要求1所述之水性防腐蚀树脂的制备方法，其特征在于，其原料范围为：55～70份环氧树脂，1～3.5份酸类物质，15～26份改性物质，25～40份有机溶剂和5～8份有机胺，70～90份去离子水。The method for preparing an aqueous anti-corrosion resin according to claim 1, wherein the raw material range is: 55 to 70 parts of an epoxy resin, 1 to 3.5 parts of an acid substance, 15 to 26 parts of a modified substance, 25 to 40 parts of organic solvent and 5-8 parts of organic amine, 70-90 parts of deionized water.
  6. 如权利要求1-5任一权利要求所述之水性防腐蚀树脂的制备方法，其特征在于：所述环氧树脂为双酚A类环氧树脂或双酚F类环氧树脂，其环氧当量范围为150～3500。The method for preparing an aqueous anti-corrosion resin according to any one of claims 1 to 5, wherein the epoxy resin is a bisphenol A epoxy resin or a bisphenol F epoxy resin, and the epoxy resin thereof The equivalent range is from 150 to 3,500.
  7. 如权利要求1-5任一权利要求所述之水性防腐蚀树脂的制备方 法，其特征在于：所述改性物质包括甲苯二异氰酸酯(TDI)、六亚甲基二异氰酸酯(HDI)、异佛尔酮二异氰酸酯(IPDI)或二苯基甲烷二异氰酸酯(MDI)，以及其加成物或三聚体，丙烯酸，甲基丙烯酸，甲基丙烯酸甲酯，丙烯酸丁酯，丙烯酸羟乙酯、苯乙烯、大豆油酸、亚麻油酸，脱水蓖麻油酸、叶子油酸、己二酸、过氧化苯甲酰中的一种或几种。Preparation method of aqueous anti-corrosion resin according to any one of claims 1 to 5 The method is characterized in that the modified substance comprises toluene diisocyanate (TDI), hexamethylene diisocyanate (HDI), isophorone diisocyanate (IPDI) or diphenylmethane diisocyanate (MDI), and An adduct or trimer thereof, acrylic acid, methacrylic acid, methyl methacrylate, butyl acrylate, hydroxyethyl acrylate, styrene, soybean oleic acid, linoleic acid, dehydrated ricinoleic acid, leaf oleic acid, One or more of adipic acid and benzoyl peroxide.
  8. 如权利要求1-5任一权利要求所述之水性防腐蚀树脂的制备方法，其特征在于：所述有机溶剂乙二醇单丁醚、丙二醇甲醚、丙二醇甲醚醋酸酯、丁醇或醇酯十二、N-甲基吡咯烷酮，二乙二醇丁醚中的一种或几种。The method for preparing an aqueous anti-corrosion resin according to any one of claims 1 to 5, wherein the organic solvent ethylene glycol monobutyl ether, propylene glycol methyl ether, propylene glycol methyl ether acetate, butanol or alcohol One or more of ester 12, N-methylpyrrolidone, diethylene glycol butyl ether.
  9. 如权利要求1-5任一权利要求所述之水性防腐蚀树脂的制备方法，其特征在于：所述酸类物质为盐酸、硫酸、磷酸、焦磷酸、多聚磷酸、柠檬酸或酒石酸中的一种或几种。The method for preparing an aqueous anti-corrosion resin according to any one of claims 1 to 5, wherein the acid substance is hydrochloric acid, sulfuric acid, phosphoric acid, pyrophosphoric acid, polyphosphoric acid, citric acid or tartaric acid. One or several.
  10. 如权利要求1-5任一权利要求所述之水性防腐蚀树脂的制备方法，其特征在于：所述有机胺为三乙胺、N,N二甲基乙醇胺或三乙醇胺中的一种或几种。 The method for preparing an aqueous anti-corrosion resin according to any one of claims 1 to 5, wherein the organic amine is one or more of triethylamine, N, N-dimethylethanolamine or triethanolamine. Kind.
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CN114318875B (en) * 2021-11-25 2023-11-10 宜兴市伟业玻纤材料有限公司 Preparation method of epoxy emulsion for corrosion-resistant high-pressure pipeline yarns
CN114657546A (en) * 2022-04-07 2022-06-24 武汉铁路职业技术学院 Anti-corrosion treatment process for railway track embedded part
CN116162248A (en) * 2022-12-30 2023-05-26 鲁东大学 Hyperbranched emulsifier for water-based heavy-duty coating resin and preparation method thereof

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CN104372317A (en) 2015-02-25
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CN104388912B (en) 2017-09-19
WO2015058683A1 (en) 2015-04-30

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