CN102516870B - Heat resistant aluminum color epoxy organosilicon paint and preparation method thereof - Google Patents

Heat resistant aluminum color epoxy organosilicon paint and preparation method thereof Download PDF

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CN102516870B
CN102516870B CN 201110432241 CN201110432241A CN102516870B CN 102516870 B CN102516870 B CN 102516870B CN 201110432241 CN201110432241 CN 201110432241 CN 201110432241 A CN201110432241 A CN 201110432241A CN 102516870 B CN102516870 B CN 102516870B
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epoxy
ingredients
water
resistance
h61
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CN 201110432241
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CN102516870A (en )
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刘建颖
王宏心
王洪鹏
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天津灯塔涂料工业发展有限公司
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Abstract

本发明涉及一种铝色环氧有机硅耐热漆,其特征是:按重量份数比,成份一:H61-1环氧改性有机硅树脂100;成份二:聚酰胺树脂80-100、甲苯40-50、丁醇40-50、环已酮10-20;成份三:浮型铝粉20;制备方法,制备H61-1环氧改性有机硅树脂;将聚酰胺树脂、甲苯、丁醇、环已酮加入配料盆中低中速200-400转/分搅拌15分钟,测固体合格后包装;浮型铝粉检验后包装;按成份一:成份二:成份三=100:30:20混合静置20分,检测后包装。 The present invention relates to an aluminum heat-resistant paint color epoxy silicone, characterized in that: parts by weight ratio of components a: H61-1 epoxy-modified silicone resin 100; two ingredients: the polyamide resin 80-100, toluene 40-50, 40-50 butanol, cyclohexanone 10-20; three ingredients: 20 leafing aluminum powder; preparation prepared H61-1 epoxy-modified silicone resin; polyamide resin, toluene, butyl alcohol, cyclohexanone was added ingredients pots low speed 200-400 rpm / min for 15 minutes, measured after passing the solid packing; leafing aluminum test after packaging; a press ingredients: ingredients two: three component = 100: 30: 20 mixture stand for 20 minutes, after detecting the packaging. 有益效果:具有优异的装饰性、耐热性、耐盐雾性、耐盐水性、耐水性、耐寒性、耐油性、耐烃类溶剂、附着力、冲击性、柔韧性等理化性能。 Advantages: excellent decorative properties, heat resistance, salt spray resistance, salt water resistance, water resistance, cold resistance, oil resistance and a hydrocarbon solvent, adhesion, impact resistance, flexibility and other physical and chemical properties.

Description

铝色环氧有机硅耐热漆及制备方法技术领域 Aluminum heat-resistant paint, and epoxy silicone TECHNICAL FIELD

[0001] 本发明属于化工涂料,尤其涉及一种铝色环氧有机硅耐热漆及制备方法。 [0001] The present invention belongs to the chemical coatings, more particularly to a heat resistant aluminum pigmented epoxy silicone paint and method of preparation.

背景技术 Background technique

[0002] 现有的环氧有机硅树脂或漆能够满足一般的装饰、耐热性和保护要求,但对特殊的性能要求如耐盐雾、耐湿热、耐寒性、耐盐水、耐滑油、耐烃类液体、耐热500°C以上等性能不能满足要求。 [0002] The conventional epoxy resin or a silicone varnish to meet the general decoration, protection and heat resistance requirements, but for special performance requirements, such as salt spray resistance, heat resistance, cold resistance, salt water resistance, oil resistance, hydrocarbon liquid, and above 500 ° C heat-resistant performance can not meet the requirements. 环氧改性有机硅树脂作为耐热漆的成膜物具有优良的耐高温性、耐大气性及耐湿热性,对金属有良好的附着力,是高温防腐、高温绝缘等特殊用途不可缺少的材料。 Epoxy-modified silicone resin as the film forming material having excellent heat-resistant paint of high temperature resistance, weathering resistance and heat resistance, good adhesion to metal, high temperature corrosion, high temperature insulation and other special purpose indispensable material. 其关键原因是市售的环氧改性有机硅树脂环氧树脂占的比例低(一般环氧:有机硅为3: The key reason is that commercial low epoxy-modified silicone resin, an epoxy resin proportion (typically epoxy: silicone-3:

7),不能满足特定产品的使用要求。 7), can not meet the requirements of a particular product. 因而限制了环氧有机硅树脂或漆的应用。 Thus limiting the use of epoxy or silicone resin paint.

发明内容 SUMMARY

[0003] 本发明是为了克服现有技术中的不足,提供一种铝色环氧有机硅耐热漆及制备方法,具有优良的耐高温性、耐大气性、耐盐雾性、耐盐水性、耐水性、耐寒性、耐油性、耐烃类溶剂、耐湿热性,附着力、冲击性、柔韧性等理化性能。 [0003] The present invention is to overcome the shortcomings of the prior art, there is provided an aluminum epoxy silicone heat-resistant paint color and the preparation method, having excellent heat resistance, weathering resistance, salt spray resistance, salt water , water resistance, cold resistance, oil resistance and a hydrocarbon solvent, moist heat resistance, adhesion, impact resistance, flexibility and other physical and chemical properties.

[0004] 本发明为实现上述目的,通过以下技术方案实现:一种铝色环氧有机硅耐热漆,其特征是:包含自制的H61-1环氧改性有机硅树脂、聚酰胺固化剂、浮型铝粉,按重量份数比 [0004] To achieve the above object of the present invention is achieved by the following technical solution: A heat-resistant aluminum color silicone epoxy varnish, characterized in that: the self-H61-1 comprising an epoxy-modified silicone resin, a polyamide curing agent , leafing aluminum powder, in parts by weight ratio of

[0005]成份一: [0005] a composition:

[0006] H61-1环氧改性有机硅树脂 100 [0006] H61-1 epoxy-modified silicone resin 100

[0007]成份二: [0007] Ingredients II:

[0008] 聚酰胺树脂 80-100 [0008] The polyamide resin 80-100

[0009]甲苯 40-50 [0009] Toluene 40-50

[0010] 丁醇 40-50 [0010] butanol 40-50

[0011]环已酮 10-20 [0011] cyclohexanone 10-20

[0012] 成份三: [0012] Ingredients III:

[0013] 浮型铝粉 20 [0013] leafing aluminum powder 20

[0014] 成份一:成份二:成份三=100:30:20 ; [0014] a composition: Ingredients two: three component = 100: 30: 20;

[0015] 其中:H61-1环氧改性有机硅树脂 [0015] wherein: H61-1 epoxy-modified silicone resin

[0016] 一甲基三氯硅烷2-15 [0016] a 2-15 methyltrichlorosilane

[0017] 二甲基二氯硅烷2-15 [0017] dimethyldichlorosilane 2-15

[0018] 一苯基三氯硅烷5-15 [0018] a phenyl trichlorosilane 5-15

[0019] 二苯基二氯硅烷2-15 [0019] diphenyldichlorosilane 2-15

[0020] 二甲苯 15-30 [0020] Xylene 15-30

[0021]乙醇 10-30 [0021] Ethanol 10-30

[0022]水 40-50 [0022] Water 40-50

[0023] 601 环氧树脂20-35[0024]环已酮 10-20 [0023] Epoxy 601 20-35 [0024] 10-20 cyclohexanone

[0025] 二甲苯 20-50。 [0025] Xylene 20-50.

[0026] 上述铝色环氧有机硅耐热漆的制备方法,其特征是:按以下步骤进行, [0026] The method for preparing the heat-resistant aluminum color epoxy silicone paint, characterized in that: the following steps performed,

[0027] 一、制备H61-1环氧改性有机硅树脂 [0027] I. Preparation of epoxy-modified silicone resin H61-1

[0028] I)将一甲基三氯硅烷、二甲基二氯硅烷、一苯基三氯硅烷、二苯基二氯硅烷及二甲苯按配方规定量加入混合罐内,搅拌均匀备用; [0028] I) to a methyltrichlorosilane, dimethyldichlorosilane, a phenyltrichlorosilane, diphenyldichlorosilane and xylene according to the formula predetermined amount into a mixing tank, stirring evenly standby;

[0029] 2)将乙醇及水按配方量加入水解釜,开动搅拌,同时夹套通冷却水,液温控制在20-30°C,开动搅拌5分钟后开始滴加上述备用混合单体,于3-4小时加完,水解温度20-30 0C ; [0029] 2) The ethanol and water added in an amount according to the formula Hydrolysis reactor, stirring was started, while the cooling water through the jacket, the liquid temperature control 20-30 ° C, start stirring for 5 minutes after starting the spare monomer mixture was added dropwise, addition was completed in 3-4 hours, the hydrolysis temperature 20-30 0C;

[0030] 3)混合单体加完后,继续搅拌5分钟,然后静置分层,放去下层酸水,上层硅醇用水进行水洗; [0030] 3) mixing the monomer addition was complete, stirring was continued for 5 minutes and then standing layer, the lower layer was acidic water discharge, the upper layer washed with water silanol water;

[0031] 4)水洗4次以上,每次水洗用水量与水解用水量相同,一直水洗到测硅醇值不大于1.5mgK0H/克为止; [0031] 4) The above washed four times with washing water hydrolysis same water, washed with water up to the silicon alcohol is not greater than the measured far 1.5mgK0H / g;

[0032] 5)将水洗合格的硅醇加入浓缩釜内,浓缩釜夹套通蒸汽升温50-70 °C,静置20-40分钟后放去釜内分出的下层水份,然后开动真空泵,减压浓缩,真空度控制在 [0032] 5) The water added to the silanol qualified concentrated kettle, the kettle was concentrated heating steam jacket to 50-70 ° C, left to stand to put the vessel in the lower layer was separated water after 20-40 minutes, and then start the vacuum pump , concentrated under reduced pressure, the degree of vacuum in the

0.03-0.06MPa,温度不能超过115°C,浓缩硅醇固体含量控制在55-65%之间,浓缩到终点后,停真空,夹套改通冷却水冷却至30-50°C放料,记录得量,并测定固体含量,准备共缩聚; After 0.03-0.06MPa, the temperature should not exceed 115 ° C, concentrated to a solids content of silanol controlled between 55-65%, is concentrated to the end, breaking the vacuum, cooling water through the jacket changed to 30-50 ° C discharge, Yield recording, and measuring the solids content, to prepare co-condensation;

[0033] 6)将按配方计算重量的浓缩硅醇加入缩聚釜并在开动搅拌状态下将已粉碎的601环氧树脂及环已酮加入缩聚釜中升温,当温度达到150-175Ό时保持回流1-2小时,当反应物料呈透明状态后升温至180°C并`保持反应,并取样于250°C下测胶化时间,当胶化时间为50-100秒作为共缩聚反应终点,立即加入二甲苯稀释,温度降至50°C测固体和粘度,合格后过滤包装; [0033] 6) will be calculated by weight of the concentrate formulation were added silanol condensation Stirring tank and a state 601 of epoxy resin, and pulverized cyclohexanone was added in the polycondensation reactor heated to maintain reflux when the temperature reaches 150-175Ό 1-2 hours. after the reaction mass was transparent and warmed to 180 ° C and maintaining the reaction `, and sampled to measure the gel time at 250 ° C, when the gel time of 50-100 seconds as a co-condensation reaction end, immediately diluted with xylene was added, the temperature dropped to 50 ° C and the viscosity measured solids, after passing the filtration packing;

[0034] 二、将成份二中的聚酰胺树脂、甲苯、丁醇、环已酮加入配料盆中低中速200-400转/分搅拌15分钟,测固体合格后包装; [0034] Second, the two components of a polyamide resin, toluene, butanol, cyclohexanone was added after formulation pots low speed 200-400 rpm / min for 15 min stirring, solid measuring qualified packing;

[0035] 三、将浮型铝粉检验后包装作为成份三; [0035] Third, after leafing aluminum test packaging as an ingredient III;

[0036] 四、将三个成份按成份一:成份二:成份三=100:30:20的配比混合均匀后静置20分钟,喷板检测各项性能,合格后包装。 [0036] Fourth, a composition according to the three components: Ingredients two: three component = 100: 30: 20 ratio to stand for 20 minutes after the mixing, the spray performance detection plate, after passing the packaging.

[0037] 有益效果:采用新的缩聚合工艺合成环氧改性有机硅树脂,优化设计配方,环氧与有机硅比例1:1,高于并优于市售同类树脂的性能,精选防锈颜料、聚酰胺树脂、溶剂及配t匕,使研制的铝色环氧有机硅耐热漆具有优异的装饰性、耐热性、耐盐雾性、耐盐水性、耐水性、耐寒性、耐油性、耐烃类溶剂、附着力、冲击性、柔韧性等理化性能。 [0037] Advantageous Effects: new condensation polymerization process for the synthesis of epoxy-modified silicone resin, design optimization formulation, the silicone epoxy ratio 1: 1, and better performance than the commercial grade resin, selection of anti rust pigment, a polyamide resin, and a solvent with t dagger, so that color development of the aluminum heat-resistant epoxy silicone paint has excellent decorative properties, heat resistance, salt spray resistance, salt water resistance, water resistance, cold resistance, oil resistance and a hydrocarbon solvent, adhesion, impact resistance, flexibility and other physical and chemical properties. H61-1环氧改性有机硅树脂中环氧树脂含量较高(环氧与有机硅比例1:1,而市售的多为3:7),与聚酰胺树脂产生交联反应满足了产品的耐各种介质性及理化性能。 H61-1 epoxy-modified silicone resin, an epoxy resin content higher (epoxy silicone ratio of 1: 1, and more commercially available 3: 7), with the polyamide resin cross-linking reaction products meet the resistance and resistance to a variety of physical and chemical properties of the medium. 同时优于市场同类产品的性能,得到用户认可。 At the same time performance is better than similar products in the market, recognized by users.

具体实施方式 detailed description

[0038] 以下结合较佳实施例,对依据本发明提供的具体实施方式详述如下。 [0038] The following embodiments in conjunction with the preferred embodiments, specific embodiments according to the present invention provides detailed below.

[0039] 实施例1[0040] 一种铝色环氧有机硅耐热漆,包含自制的H61-1环氧改性有机硅树脂、聚酰胺固化剂、浮型铝粉,按重量计(g) [0039] Example 1 [0040] A heat-resistant aluminum pigmented silicone epoxy varnish, homemade H61-1 comprising an epoxy-modified silicone resin, a polyamide curing agent, a leafing aluminum powder, by weight, (g )

[0041]成份一: [0041] a composition:

[0042] H61-1环氧改性有机硅树脂 100 [0042] H61-1 epoxy-modified silicone resin 100

[0043]成份二: [0044] 聚酰胺树脂 80-100 [0043] component II: [0044] a polyamide resin 80-100

[0045]甲苯 40-50 [0045] Toluene 40-50

[0046] 丁醇 40-50 [0046] butanol 40-50

[0047]环已酮 10-20 [0047] cyclohexanone 10-20

[0048] 成份三: [0048] Ingredients III:

[0049] 浮型铝粉 20 [0049] leafing aluminum powder 20

[0050] 成份一:成份二:成份三=100:30:20 ; [0050] a composition: Ingredients two: three component = 100: 30: 20;

[0051] 其中:H61-1环氧改性有机硅树脂 [0051] wherein: H61-1 epoxy-modified silicone resin

[0052] 一甲基三氯硅烷2-15 [0052] a 2-15 methyltrichlorosilane

[0053] 二甲基二氯硅烷2-15 [0053] dimethyldichlorosilane 2-15

[0054] 一苯基三氯硅烷5-15 [0054] a phenyl trichlorosilane 5-15

[0055] 二苯基二氯硅烷2-15 [0055] diphenyldichlorosilane 2-15

[0056] 二甲苯 15-30 [0056] Xylene 15-30

[0057]乙醇 10-30 [0057] Ethanol 10-30

[0058]水 40-50 [0058] Water 40-50

[0059] 601 环氧树脂20-:35 [0059] Epoxy 601 20: 35

[0060]环已酮 10-20 [0060] cyclohexanone 10-20

[0061] 二甲苯 20-50。 [0061] Xylene 20-50.

[0062] 实施例2 [0062] Example 2

[0063] 一种铝色环氧有机硅耐热漆,包含自制的H61-1环氧改性有机硅树脂、聚酰胺固化剂、浮型铝粉,按重量计(g) [0063] A heat-resistant aluminum pigmented silicone epoxy varnish, homemade H61-1 comprising an epoxy-modified silicone resin, a polyamide curing agent, a leafing aluminum powder by weight (g)

[0064]成份一: [0064] a composition:

[0065] H61-1环氧改性有机硅树脂 100 g [0065] H61-1 epoxy-modified silicone resin 100 g

[0066]成份二: [0066] Ingredients II:

[0067] 聚酰胺树脂 80 g [0067] 80 g of the polyamide resin

[0068]甲苯 40 g [0068] 40 g of toluene

[0069] 丁醇 40 g [0069] 40 g Butanol

[0070] 环已酮 10 g [0070] 10 g of cyclohexanone

[0071] 成份三: [0071] The three ingredients:

[0072] 浮型铝粉 20 g [0072] 20 g leafing aluminum powder

[0073] 成份一:成份二:成份三=100:30:20 ; [0073] a composition: Ingredients two: three component = 100: 30: 20;

[0074] 其中:H61-1环氧改性有机硅树脂 [0074] wherein: H61-1 epoxy-modified silicone resin

[0075] 一甲基三氯硅烷2 g [0075] 2 g of methyltrichlorosilane a

[0076] 二甲基二氯硅烷2 g[0077] 一苯基三氯硅烷5 g [0076] dimethyldichlorosilane 2 g [0077] a 5 g phenyltrichlorosilane

[0078] 二苯基二氯硅烷2 g [0078] 2 g diphenyldichlorosilane

[0079] 二甲苯 15 g [0079] 15 g of xylene

[0080]乙醇 10 g [0080] 10 g of ethanol

[0081]水 40 g [0081] Water 40 g

[0082] 601环氧树脂20 g [0082] 20 g of epoxy resin 601

[0083] 环已酮 10 g [0083] 10 g of cyclohexanone

[0084] 二甲苯 20 g。 [0084] p-xylene 20 g.

[0085] 实施例3 [0085] Example 3

[0086] 一种铝色环氧有机硅耐热漆,包含自制的H61-1环氧改性有机硅树脂、聚酰胺固化剂、浮型铝粉组成,按重量计(g ) [0086] A heat-resistant aluminum pigmented silicone epoxy varnish, homemade H61-1 comprising an epoxy-modified silicone resin, a polyamide curing agent, a leafing aluminum powder by weight (g)

[0087]成份一: [0088] H61-1环氧改性有机硅树脂 100 g [0087] a composition: [0088] H61-1 epoxy-modified silicone resin 100 g

[0089]成份二: [0089] Ingredients II:

[0090] 聚酰胺树脂 100 g [0090] 100 g of the polyamide resin

[0091]甲苯 50 g [0091] 50 g of toluene

[0092] 丁醇 50 g [0092] 50 g Butanol

[0093] 环已酮 20 g [0093] 20 g of cyclohexanone

[0094]成份二: [0094] Ingredients II:

[0095] 浮型铝粉 20 g [0095] 20 g leafing aluminum powder

[0096] 成份一:成份二:成份三=100:30:20 ; [0096] a composition: Ingredients two: three component = 100: 30: 20;

[0097] 其中:H61-1环氧改性有机硅树脂 [0097] wherein: H61-1 epoxy-modified silicone resin

[0098] 一甲基三氯硅烷15 g [0098] 15 g of methyltrichlorosilane a

[0099] 二甲基二氯硅烷15 g [0099] 15 g of dimethyldichlorosilane

[0100] 一苯基三氯硅烷15 g [0100] 15 g of phenyltrichlorosilane a

[0101] 二苯基二氯硅烷15 g [0101] 15 g diphenyldichlorosilane

[0102] 二甲苯 30 g [0102] 30 g of xylene

[0103]乙醇 30 g [0103] 30 g of ethanol

[0104]水 50 g [0104] Water 50 g

[0105] 601环氧树脂35 g [0105] 35 g of epoxy resin 601

[0106] 环已丽 20 g [0106] 20 g cyclohexanone Korea

[0107] 二甲苯 50 g。 [0107] Xylene 50 g.

[0108] 实施例4 [0108] Example 4

[0109] 一种铝色环氧有机硅耐热漆,包含自制的H61-1环氧改性有机硅树脂、聚酰胺固化剂、浮型铝粉,按重量计(g) [0109] A heat-resistant aluminum pigmented silicone epoxy varnish, homemade H61-1 comprising an epoxy-modified silicone resin, a polyamide curing agent, a leafing aluminum powder by weight (g)

[0110]成份一: [0110] a composition:

[0111] H61-1环氧改性有机硅树脂 100g [0111] H61-1 epoxy-modified silicone resin 100g

[0112]成份二: [0112] Ingredients II:

[0113] 聚酰胺树脂 85 g[0114]甲苯 45 g [0113] The polyamide resin is 85 g [0114] 45 g of toluene

[0115] 丁醇 45 g [0115] 45 g Butanol

[0116] 环已酮 15 g [0116] 15 g of cyclohexanone

[0117] 成份三: [0117] Ingredients III:

[0118] 浮型铝粉 20 g [0118] 20 g leafing aluminum powder

[0119] 成份一:成份二:成份三=100:30:20 ; [0119] a composition: Ingredients two: three component = 100: 30: 20;

[0120] 其中:H61-1环氧改性有机硅树脂 [0120] wherein: H61-1 epoxy-modified silicone resin

[0121] 一甲基三氯硅烷10 g [0121] 10 g of methyltrichlorosilane a

[0122] 二甲基二氯硅烷5 g [0122] 5 g of dimethyldichlorosilane

[0123] 一苯基三氯硅烷10 g [0123] 10 g of phenyltrichlorosilane a

[0124] 二苯基二氯硅烷10 g [0124] 10 g diphenyldichlorosilane

[0125] 二甲苯 20 g [0125] 20 g of xylene

[0126]乙醇 15 g [0126] 15 g of ethanol

[0127]水 45 g [0127] Water 45 g

[0128] 601环氧树脂25 g [0128] 25 g of epoxy resin 601

[0129] 环已酮 15 g [0129] 15 g of cyclohexanone

[0130] 二甲苯 25 g。 [0130] p-xylene 25 g.

[0131] 实施例5 [0131] Example 5

[0132] 一种铝色环氧有机硅耐热漆,包含自制的H61-1环氧改性有机硅树脂、聚酰胺固化剂、浮型铝粉,按重量计(g) [0132] A heat-resistant aluminum pigmented silicone epoxy varnish, homemade H61-1 comprising an epoxy-modified silicone resin, a polyamide curing agent, a leafing aluminum powder by weight (g)

[0133]成份一: [0133] a composition:

[0134] H61-1环氧改性有机硅树脂 100g [0134] H61-1 epoxy-modified silicone resin 100g

[0135]成份二: [0135] Ingredients II:

[0136] 聚酰胺树脂 90 g [0136] 90 g of the polyamide resin

[0137]甲苯 40 g [0137] 40 g of toluene

[0138] 丁醇 50 g [0138] 50 g Butanol

[0139]环已酮 10 g [0139] 10 g of cyclohexanone

[0140]成份二: [0140] Ingredients II:

[0141] 浮型铝粉 20 g [0141] 20 g leafing aluminum powder

[0142] 成份一:成份二:成份三=100:30:20 ; [0142] a composition: Ingredients two: three component = 100: 30: 20;

[0143] 其中:H61-1环氧改性有机硅树脂 [0143] wherein: H61-1 epoxy-modified silicone resin

[0144] 一甲基三氯硅烷2 g [0144] 2 g of methyltrichlorosilane a

[0145] 二甲基二氯硅烷15 g [0145] 15 g of dimethyldichlorosilane

[0146] 一苯基三氯硅烷5 g [0146] a 5 g phenyltrichlorosilane

[0147] 二苯基二氯硅烷15 g [0147] 15 g diphenyldichlorosilane

[0148] 二甲苯 15 g [0148] 15 g of xylene

[0149]乙醇 10 g [0149] 10 g of ethanol

[0150]水 50 g [0150] Water 50 g

[0151] 601环氧树脂20 g[0152] 环已酮 10 g [0151] Epoxy 601 20 g [0152] 10 g of cyclohexanone

[0153] 二甲苯 3 O g。 [0153] Xylene 3 O g.

[0154] 上述铝色环氧有机硅耐热漆的制备方法,按以下步骤进行, [0154] The method of preparing the above-described heat-resistant aluminum color epoxy silicone paint, perform the following steps,

[0155] 一、制备H61-1环氧改性有机硅树脂 [0155] I. Preparation of epoxy-modified silicone resin H61-1

[0156] I)将一甲基三氯硅烷、二甲基二氯硅烷、一苯基三氯硅烷、二苯基二氯硅烷及二甲苯按配方规定量加入混合罐内,搅拌均匀备用; [0156] I) to a methyltrichlorosilane, dimethyldichlorosilane, a phenyltrichlorosilane, diphenyldichlorosilane and xylene according to the formula predetermined amount into a mixing tank, stirring evenly standby;

[0157] 2)将乙醇及水按配方量加入水解釜,开动搅拌,同时夹套通冷却水,液温控制在20-30°C,开动搅拌5分钟后开始滴加上述备用混合单体,于3-4小时加完,水解温度20-30 0C ; [0157] 2) The ethanol and water added in an amount according to the formula Hydrolysis reactor, stirring was started, while the cooling water through the jacket, the liquid temperature control 20-30 ° C, start stirring for 5 minutes after starting the spare monomer mixture was added dropwise, addition was completed in 3-4 hours, the hydrolysis temperature 20-30 0C;

[0158] 3)混合单体加完后,继续搅拌5分钟,然后静置分层,放去下层酸水,上层硅醇用水进行水洗; [0158] 3) mixing the monomer addition was complete, stirring was continued for 5 minutes and then standing layer, the lower layer was acidic water discharge, the upper layer washed with water silanol water;

[0159] 4)水洗4次以上,每次水洗用水量与水解用水量相同,一直水洗到测硅醇值不大于1.5mgK0H/克为止; [0159] 4) The above washed four times with washing water hydrolysis same water, washed with water up to the silicon alcohol is not greater than the measured far 1.5mgK0H / g;

[0160] 5)将水洗合格的硅醇加入浓缩釜内,浓缩釜夹套通蒸汽升温50-70 °C,静置20-40分钟后放去釜内分出的下层水份,然后开动真空泵,减压浓缩,真空度控制在 [0160] 5) The water added to the silanol qualified concentrated kettle, the kettle was concentrated heating steam jacket to 50-70 ° C, left to stand to put the vessel in the lower layer was separated water after 20-40 minutes, and then start the vacuum pump , concentrated under reduced pressure, the degree of vacuum in the

0.03-0.06MPa,温度不能超过115°C,浓缩硅醇固体含量控制在55-65%之间,浓缩到终点后,停真空,夹套改通冷却水冷却至30-50°C放料,记录得量,并测定固体含量,准备共缩聚; After 0.03-0.06MPa, the temperature should not exceed 115 ° C, concentrated to a solids content of silanol controlled between 55-65%, is concentrated to the end, breaking the vacuum, cooling water through the jacket changed to 30-50 ° C discharge, Yield recording, and measuring the solids content, to prepare co-condensation;

[0161] 6)将按配方计算重量的浓缩硅醇加入缩聚釜并在开动搅拌状态下将已粉碎的601环氧树脂及环已酮加入缩聚釜中升温,`当温度达到150-175Ό时保持回流1-2小时,当反应物料呈透明状态后升温至180°C并保持反应,并取样于250°C下测胶化时间,当胶化时间为50-100秒作为共缩聚反应终点,立即加入二甲苯稀释,温度降至50°C测固体和粘度,合格后过滤包装; [0161] 6) will be calculated by weight of the concentrate formulation were added silanol condensation Stirring tank and a state of pulverized 601 epoxy was added, and the polycondensation of cyclohexanone heated kettle, `maintained when the temperature reaches 150-175Ό reflux 1-2 hours. after the reaction mass was transparent and warmed to 180 ° C and maintaining the reaction, and sampled to measure the gel time at 250 ° C, when the gel time of 50 to 100 seconds as the co-condensation reaction end point, immediately diluted with xylene was added, the temperature dropped to 50 ° C and the viscosity measured solids, after passing the filtration packing;

[0162] 二、将成份二中的聚酰胺树脂、甲苯、丁醇、环已酮加入配料盆中低中速200-400转/分搅拌15分钟,测固体合格后包装; [0162] Second, the two components of a polyamide resin, toluene, butanol, cyclohexanone was added after formulation pots low speed 200-400 rpm / min for 15 min stirring, solid measuring qualified packing;

[0163] 三、将浮型铝粉检验后包装作为成份三; [0163] Third, after leafing aluminum test packaging as an ingredient III;

[0164] 四、将三个成份按成份一:成份二:成份三=100:30:20的配比混合均匀后静置20分钟,喷板检测各项性能,合格后包装。 [0164] Fourth, a composition according to the three components: Ingredients two: three component = 100: 30: 20 ratio to stand for 20 minutes after the mixing, the spray performance detection plate, after passing the packaging.

[0165] H61-1环氧改性有机硅树脂的特点: [0165] H61-1 epoxy-modified silicone resin characteristics:

[0166] 该树脂由环氧树脂与有机硅醇1:1缩聚而成,兼具了环氧树脂附着力好、固化后的涂膜耐腐蚀性和耐化学药品性能优异、涂膜收缩小、硬度高、耐磨性好、电气绝缘性能优异等性能及有机硅树脂优良的耐热性、电绝缘性、耐高温、耐低温、耐电晕、耐潮湿和抗水性。 [0166] The silicone resin is an epoxy resin with an organic alcohol 1: 1 condensation formed, both the epoxy good adhesion, coating film excellent in corrosion resistance and chemical resistance after curing, small coated film shrinkage, high hardness, good wear resistance, excellent electrical insulation properties and excellent heat resistance silicone resin, electrically insulating, high temperature, low temperature, corona resistance, moisture resistance and water resistance. 它的耐高温性幅度在150°C-700°C。 Its high temperature range of 150 ° C-700 ° C. 自制的H61-1环氧改性有机硅树脂可以加入铝粉做成具有防腐性的铝色环氧有机硅耐热漆,也可加入其他防腐颜料、耐高温颜料制备各色环氧有机硅防腐耐热漆,其综合性能优于市售树脂,满足产品及用户的使用要求。 Homemade H61-1 epoxy-modified silicone resin may be made of aluminum powder added aluminum color epoxy silicone having anticorrosive heat-resistant paint, may be added to other anticorrosive pigments, color pigments prepared in high temperature corrosion resistant epoxy silicone hot paint, its overall performance is better than the commercially available resins, and products meet the requirements of users.

[0167] 关键技术指标: [0167] key technical indicators:

[0168]粘度,S [0168] Viscosity, S

[0169]成分一 15-45 [0169] a component 15-45

[0170]成分二 10-30[0171] 干燥时间,h 不大于 [0170] two component 10-30 [0171] Drying Time, h is not greater than

[0172]表干(23±2°C) 8 [0172] dry (23 ± 2 ° C) 8

[0173]实干(23±2°C) 24 [0173] hard work (23 ± 2 ° C) 24

[0174]烘干(120±5°C) 4 [0174] Drying (120 ± 5 ° C) 4

[0175] 附着力,级不大于 I [0175] Adhesion level is not greater than I

[0176] 柔韧性,_ 2 [0176] flexibility, _ 2

[0177]冲击性,cm 50 [0177] impact resistance, cm 50

[0178] 耐热性(500±10°C),10h 漆膜不破裂、允许失光变色,冲击性通过15cm [0178] heat resistance (500 ± 10 ° C), 10h film does not rupture, allowing loss of light color, impact resistance by 15cm

[0179] 耐湿热性,168h,级 I [0179] moist heat resistance, 168h, Class I

[0180] 耐寒性(-50±5°C),lh 漆膜完整 [0180] cold (-50 ± 5 ° C), lh complete paint

[0181] 耐盐雾性(耐热300°C IOh[0182] 后耐盐雾12h) 漆膜不起泡,不脱落。 [0181] Salt spray resistance (300 ° C IOh after heat [0182] resistance to salt spray 12h) the film does not blister, do not fall off.

[0183] 耐水性,24h 不起泡,不脱落,允许轻微变色 [0183] Water resistance, 24h no blistering, no loss, allowing a slight discoloration

[0184] 耐盐水性,(3%NaCL) 24h 不起泡,不脱落,允许轻微变色 [0184] salt water, (3% NaCL) 24h no blistering, no loss, allowing a slight discoloration

[0185] 耐烃类液体,4h 不起皱,不起泡,附着力I级 [0185] Resistance of a hydrocarbon liquid, 4h crease, foaming, adhesion level I

[0186] 耐滑油(150±2°C)24h 不起皱,不起泡,不脱落。 [0186] Oil resistance (150 ± 2 ° C) 24h not wrinkle, no blistering, no loss.

[0187] 以上所述,仅是本发明的较佳实施例而已,并非对本发明的结构作任何形式上的限制。 [0187] The above, only the preferred embodiment of the present invention, but not form any limitation to the structure of the present invention. 凡是依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均仍属于本发明的技术方案的范围内。 Where any simple modifications based on the technical essence of the present invention is made to the above embodiment of the embodiment, modifications and equivalent, are still within the scope of the technical solutions of the present invention.

Claims (1)

  1. 1.一种铝色环氧有机硅耐热漆的制备方法,其特征是:按以下步骤进行,包含自制的H61-1环氧改性有机硅树脂、聚酰胺固化剂、浮型铝粉,按重量份数比成份一: H61-1环氧改性有机硅树脂100 成份二: A method for producing an aluminum color epoxy silicone heat-resistant paint, characterized in that: the following steps performed, homemade H61-1 comprising an epoxy-modified silicone resin, a polyamide curing agent, a leafing aluminum powder, ingredients in parts by weight ratio of a: H61-1 epoxy-modified silicone resin component two 100:
    Figure CN102516870BC00021
    成份一:成份二:成份三=IOO:30:20 ; 其中:H61-1环氧改性有机硅树脂 A Ingredients: two ingredients: Ingredients three = IOO: 30: 20; wherein: H61-1 epoxy-modified silicone resin
    Figure CN102516870BC00022
    一、制备H61-1环氧改性有机硅树脂1)将一甲基三氯硅烷、二甲基二氯硅烷、一苯基三氯硅烷、二苯基二氯硅烷及二甲苯按配方规定量加入混合罐内,搅拌均匀备用; 2)将乙醇及水按配方量加入水解釜,开动搅拌,同时夹套通冷却水,液温控制在20-30 °C,开动搅拌5分钟后开始滴加上述备用混合单体,于3-4小时加完,水解温度20-30 0C ; 3)混合单体加完后,继续搅拌5分钟,然后静置分层,放去下层酸水,上层硅醇用水进行水洗; 4)水洗4次以上,每次水洗用水量与水解用水量相同,一直水洗到测硅醇值不大于1.5mgKOH/ 克为止; 5)将水洗合格的硅醇加入浓缩釜内,浓缩釜夹套通蒸汽升温50-70°C,静置20-40分钟后放去釜内分出的下层水份,然后开动真空泵,减压浓缩,真空度控制在0.03-0.06MPa,温度不能超过115°C,浓缩硅醇固体含量控制在55-65%之间,浓缩到终点后, I. Preparation of epoxy-modified silicone resin H61-1 1) a methyltrichlorosilane, dimethyldichlorosilane, a phenyltrichlorosilane, diphenyldichlorosilane, and a predetermined amount of xylene according to formula into a mixing tank, stirring evenly standby; 2) ethanol and water added in an amount according to the formula hydrolysis reactor, stirring was started, while the cooling water through the jacket, the liquid temperature control 20-30 ° C, dropwise addition stirring was started after 5 minutes the spare monomer mixture addition was complete in 3-4 hours, the hydrolysis temperature 20-30 0C; 3) mixing the monomer addition was complete, stirring was continued for 5 minutes and then standing layer, the lower layer was acidic water discharge, the upper silanol washing with water; 4) washed four more times, each time water washing the same with the hydrolysis water, washed with water up to the silicon alcohol measurement is not greater than 1.5mgKOH / g up; 5) passing the washed alcohol was added to the concentrated silicon kettle, steam jacketed kettle was concentrated through heating 50-70 ° C, left to stand to put the vessel in the lower layer was separated water after 20-40 minutes, then start the vacuum pump, and concentrated under reduced pressure, the degree of vacuum in 0.03-0.06MPa, temperature can not exceeds 115 ° C, the silanol solids content between 55-65% in the control, to the end and concentrated concentrated 真空,夹套改通冷却水冷却至30-50°C放料,记录得量,并测定固体含量,准备共缩聚; 6)将按配方计算重量的浓缩硅醇加入缩聚釜并在开动搅拌状态下将已粉碎的601环氧树脂及环己酮加入缩聚釜中升温,当温度达到150-175Ό时保持回流1-2小时,当反应物料呈透明状态后升温至180°C并保持反应,并取样于250°C下测胶化时间,当胶化时间为50-100秒作为共缩聚反应终点,立即加入二甲苯稀释,温度降至50°C测固体和粘度,合格后过滤包装; 二、将成份二中的聚酰胺树脂、甲苯、丁醇、环己酮加入配料盆中低中速200-400转/分搅拌15分钟,测固体合格后包装; 三、将浮型铝粉检验后包装作为成份三; 四、将三个成份按成份一:成份二:成份三=100:30:20的配比混合均匀后静置20分钟,喷板检测各项性能,合格后包装。 Vacuum, cooling water through the jacket changed to 30-50 ° C discharge, the recording yield and the determination of the solid content, to prepare copolycondensation; 6) will be calculated by weight of the concentrate formulation were added silanol condensation reactor and stirring was started state the pulverized at 601 epoxy resin, and cyclohexanone was added in the polycondensation reactor at an elevated temperature when the temperature reaches 150-175Ό reflux for 1-2 hours. after the reaction mass was transparent and warmed to 180 ° C and maintaining the reaction, and gel time measured in sampling at 250 ° C, when the gel time of 50 to 100 seconds as the co-condensation reaction end, immediately diluted xylene, temperature was lowered to 50 ° C and the viscosity measured solids, after passing the filtration packing; II. the two components of the polyamide resin, toluene, butanol, cyclohexanone was added ingredients pots low speed 200-400 rpm / min for 15 min stirring, the solid measured after passing packing; Third, after leafing aluminum packaging test as component III; four, the three components by a composition: 20 mixing ratio even after 20 minutes of standing, the discharge performance of the detection plate, after passing the packaging: ingredients two: three component = 100: 30.
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