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Preparation process for preparing mineral oil-based aluminum-oxygen polymer by using dihydroxyl aluminum carboxylate intermediate

A technology of dihydroxycarboxylic acid and aluminum hydroxycarboxylate, which is applied in the field of preparation of mineral oil-based aluminum-oxygen polymers, can solve problems such as difficult control of alumina and block particles, difficult reaction, and consumption of organic acids , to achieve the effects of easy control of reaction conditions, stable performance and high yield

Active Publication Date: 2014-12-17
浙江省中明化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the process of method 1, aluminum hydroxycarboxylate will be produced, which will form a gel in the base oil and make the reaction difficult. Therefore, the method is to first react in toluene solvent to form aluminum-oxygen polymer or aluminum-oxygen trimer, and then add Distill toluene from base oil (US2925430); although method 2 can be obtained by direct reaction in base oil, it consumes 1 equivalent of organic acid and produces ester by-products, which increases the cost (EP0029589A2)
Our unit reported in "Contemporary Chemical Industry" 2011, 40 (11): 1143-1145 and invention patent (application number CN201310154488.9) that aluminum alkoxide reacted with carboxylic acid to form an intermediate, and then reacted with water at high temperature to obtain mineral oil Based on aluminum-oxygen polymers, but the reaction of adding water at high temperature is violent, it is difficult to control and it is easy to generate alumina and blocky particles
[0005] Using method 1 has obvious economic advantages, but it uses toluene as a solvent, which will lead to toluene in the final product, which is what we don't want to see

Method used

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  • Preparation process for preparing mineral oil-based aluminum-oxygen polymer by using dihydroxyl aluminum carboxylate intermediate
  • Preparation process for preparing mineral oil-based aluminum-oxygen polymer by using dihydroxyl aluminum carboxylate intermediate
  • Preparation process for preparing mineral oil-based aluminum-oxygen polymer by using dihydroxyl aluminum carboxylate intermediate

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Add 204g of aluminum isopropoxide to 200g of isopropanol, stir and heat to 60°C, add 144g of isooctanoic acid, stir for 1 hour; add 45g of water, carry out hydrolysis reaction, keep warm at 60°C for 2 hours; filter to obtain a white precipitate , and dried to obtain 203 g (99.5% yield) of aluminum dihydroxyisooctoate powder.

[0027] Take 102g of aluminum isopropoxide and add it to 100g of mineral oil, heat to 85°C, and start to add 72g of isooctanoic acid dropwise; after dropping isocaprylic acid, heat up to 150°C; add 102g of aluminum dihydroxyisooctanoate powder, and keep warm at 140°C React for 3 hours until the solution becomes clear; cool to obtain 285 g grass-green viscous substance with an aluminum content of 9.4% and a yield of 99.6%.

Embodiment 2

[0029] Add 204g of aluminum isopropoxide to 200g of isopropanol, stir and heat to 70°C, add 284g of isooctanoic acid, stir and react for 1 hour; add 50g of water, carry out hydrolysis reaction, keep the reaction at 65°C for 2 hours; filter to obtain white precipitate , and dried to obtain 342g (99.4% yield) of aluminum dihydroxystearate powder.

[0030] Take 102g of aluminum isopropoxide and add it to 100g of mineral oil, heat to 90°C, start to add 72g of isooctanoic acid dropwise; after adding isocaprylic acid dropwise, heat up to 140°C; add 102g of aluminum dihydroxyisooctanoate powder, and keep warm at 160°C React for 8 hours until the solution is clear; cool to obtain 285 g grass green viscous liquid, the aluminum content is 9.4%, and the yield is 99.6%.

Embodiment 3

[0032] Add 204g of aluminum isopropoxide to 200g of isopropanol, stir and heat to 70°C, add 144g of isooctanoic acid, stir for 1 hour; add 45g of water, carry out hydrolysis reaction, keep the reaction at 70°C for 2 hours; filter to obtain a white precipitate , and dried to obtain 203 g (99.5% yield) of aluminum dihydroxyisooctoate powder.

[0033] Take 102g of aluminum isopropoxide and add it to 100g of mineral oil, heat to 85°C, start to add 72g of isooctanoic acid dropwise; after adding isocaprylic acid dropwise, heat up to 180°C; add 102g of aluminum dihydroxyisooctanoate powder, and keep warm at 170°C React for 2 hours until the solution is clear; cool to obtain 285 g grass green viscous liquid, the aluminum content is 9.4%, and the yield is 99.6%.

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Abstract

The invention provides a preparation process for preparing a mineral oil-based aluminum-oxygen polymer by using a dihydroxyl aluminum carboxylate intermediate. The aluminum-oxygen polymer comprises an aluminum-oxygen tripolymer. The preparation process comprises the following steps: firstly, preparing dihydroxyl aluminum carboxylate powder by taking aluminum isopropoxide, water and carboxylic acid as main raw materials; and then, heating aluminum isopropoxide and mineral oil to 140-180 DEG C and adding the dihydroxyl aluminum carboxylate powder in a corresponding amount to prepare the aluminum-oxygen polymer. The molar ratio of dihydroxyl aluminum carboxylate to aluminum isopropoxide is 1 to 1. Different from the conventional one-pot method, the preparation process provided by the invention adopts a two-pot method in which the dihydroxyl aluminum carboxylate powder is prepared firstly; therefore, the gelatinization problem caused when water is added to the mineral oil at a low temperature and the different control problem caused when water is added at a high temperature are solved, so that the dihydroxyl aluminum carboxylate powder can react stably in a reaction system which takes the mineral oil as a solvent. The preparation process is simple in method, has no special requirements for reaction equipment and has the advantages of easy control in the reaction condition, high yield and acquisition of a clear and stable finished product.

Description

technical field [0001] The invention relates to the technical field of ink gel preparation, in particular to a preparation process for preparing a mineral oil-based aluminum-oxygen polymer with an aluminum dihydroxycarboxylate intermediate. Background technique [0002] Mineral oil-based aluminum-oxygen polymers and aluminum-oxygen trimers are important types of gelling agents in the ink industry. There are two general production processes for this type of gel, and the reaction equation is: [0003] [0004] In the process of method 1, aluminum hydroxycarboxylate will be produced, which will form a gel in the base oil and make the reaction difficult. Therefore, the method is to first react in toluene solvent to form aluminum-oxygen polymer or aluminum-oxygen trimer, and then add Toluene is distilled from base oil (US2925430); although method 2 can be obtained by direct reaction in base oil, it consumes 1 equivalent of organic acid and produces ester by-products, which i...

Claims

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Application Information

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IPC IPC(8): C08G79/10C07F5/06C09D11/00
Inventor 孙云辉翁齐菲王兴隆李齐春
Owner 浙江省中明化工科技有限公司
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