Preparation method of dibasic acid of higher fatty acid and rosin resin acid

A technology of higher fatty acid and rosin resin acid, applied in the production of fatty acid, chemical modification of fatty acid, chemical modification of natural resin, etc., can solve the problems of low hardness, poor mutual solubility of epoxy resin, poor heat resistance of polyamide resin, etc.

Inactive Publication Date: 2009-12-09
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the shortcomings of polyamide resins prepared from dibasic acids or dimer acids in the prior art, which have good flexibility, poor heat resistance, low hardness, and poor miscibility with epoxy resins, the invention provides a higher fatty acid and rosin The preparation method of the dibasic acid of resin acid, the polyamide resin prepared by using the dibasic acid as raw material, has good miscibility with epoxy resin and high hardness

Method used

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  • Preparation method of dibasic acid of higher fatty acid and rosin resin acid
  • Preparation method of dibasic acid of higher fatty acid and rosin resin acid

Examples

Experimental program
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Effect test

Embodiment 1

[0032] dibasic acid of eucalyptus oleic acid and rosin resin acid

[0033] (1) Preparation of eucalyptus oleic acid

[0034] In an autoclave equipped with a stirring device and a thermometer, add 100 grams of eucalyptus seed oil, 0.5 grams of zinc oxide and 70 grams of water, stir evenly, heat to 180 ° C, and react for 4-8 hours. After the reaction, cool down to 60-90°C and neutralize with sulfuric acid to pH 3-5. The water in the lower layer was separated, and the oleic acid layer was washed to neutral, and the water in the lower layer was separated. Distill and dehydrate under the condition of 100-120°C / 1-15mmHg to obtain 90 grams of fatty acid for the next step of polymerization.

[0035] (2) Polymerization reaction:

[0036] In an autoclave equipped with a stirring device and a thermometer, add 50-95 grams of glabra oleic acid, 5-50 grams of rosin, 3-10 grams of lithium carbonate and 15-30 grams of activated clay to maintain a pressure of 0.4-1.0 MPa At 200°C-280°C, ca...

Embodiment 2

[0038] Dibasic acid of soybean oil and rosin resin acid

[0039] (1) Hydrolysis of soybean oil

[0040] In an autoclave equipped with a stirring device and a thermometer, add 100 grams of soybean oil, 0.5 grams of zinc oxide and 70 grams of water, stir evenly, heat to 180° C., and react for 4-8 hours. After the reaction, cool down to 60-90°C and neutralize with sulfuric acid to pH 3-5. The water in the lower layer was separated, and the oleic acid layer was washed to neutral, and the water in the lower layer was separated. Distill and dehydrate under the condition of 100-120°C / 1-15mmHg to obtain 90 grams of fatty acid for the next step of polymerization.

[0041] (2) Polymerization reaction:

[0042] In an autoclave equipped with a stirring device and a thermometer, add 50-95 grams of the above-mentioned oleic acid, 5-50 grams of rosin, 3-10 grams of manganese acetate and 15-30 grams of montmorillonite, and maintain a pressure of 0.4-1.0 MPa , carry out polymerization reac...

Embodiment 3

[0044] Diacids of Oleic Acid and Rosin Resin Acid Prepared from Tung Oil

[0045] (1) Hydrolysis reaction of tung oil

[0046]In an autoclave equipped with a stirring device and a thermometer, add 100 grams of tung oil, 0.5 grams of magnesium oxide and 60 grams of water, stir evenly, heat to 170 ° C, and react for 4-8 hours. After the reaction, cool down to 60-90°C and neutralize to pH 3-5 with phosphoric acid. The lower layer of water is divided, and then the tung oil layer is washed to neutrality, and the lower layer of water is separated. Distill and dehydrate under the condition of 100-110° C. / 1-15 mmHg to obtain 90 grams of fatty acid for the next step of polymerization.

[0047] (2) Polymerization reaction:

[0048] In an autoclave equipped with a stirring device and a thermometer, add 50-95 grams of eutrophic acid, 5-50 grams of rosin, 3-10 grams of iodine and 15-30 grams of activated clay. Polymerize at -280°C for 3-6 hours, cool to 80°C; measure the pH of the syst...

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Abstract

The invention discloses a preparation method of dibasic acid of higher fatty acid and rosin resin acid, comprising the following steps: step 1, appropriate grease is heated up to 150-190 DEG C, which is then catalyzed and hydrolyzed with high pressure to obtain fatty acid used for polymerization reaction; and step 2, the above higher fatty acid and appropriate rosin are premixed and added with a catalyst and a promoter, so that the mixed system is maintained at the pressure of 0.4-1.0MPa, then polymerization addition is carried out at 200-280 DEG C to obtain the required novel dibasic acid. Compared with versamid prepared by ordinary dimer acid, the versamid firming agent synthesized by the novel dibasic acid of the invention has better miscibility with epoxy resin due to the addition of the alicyclic structure of rosin, and the epoxy resin solidifying material has higher mechanical properties of compression strength, modulus of compressibility, bending strength, bending modulus and the like. The invention takes biomass resource grease and rosin as materials, having the biological degradability with which the petrified materials are not provided.

Description

1. Technical field [0001] The invention relates to a raw material for preparing polyamide resin, in particular to a method for preparing a dibasic acid of higher fatty acid and rosin resin acid. 2. Background technology [0002] Dimer acid is an important oleochemical. It is a dibasic carboxylic acid formed from unsaturated fatty acids in natural oils and fats such as oleic acid and linoleic acid through catalytic polymerization of two or more higher unsaturated fatty acid molecules. It is mainly used in the production of polyamide resin, and polyamide resin is divided into two categories: reactive type and non-reactive type. Reactive polyamide resin is prepared by the amidation reaction of dimer acid and polyamine, and is often used as a curing agent for epoxy resin. Due to the long fatty acid carbon chain and amino group in the structure, the cured product has good flexibility, adhesion, flexibility and water resistance, and can be made into coatings, adhesives, injectio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C11C3/00C09F1/04
Inventor 夏建陵杨小华陈瑶黄坤
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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