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Preparation method of long-chain star-shaped branching agent and high-fluidity high-crystallinity long-carbon-chain star-shaped polyamide

A branching agent and long carbon chain technology, applied in the field of star-shaped polyamide material preparation, can solve the problems of decreased toughness and impact strength, decreased crystallinity, low crystallinity, etc.

Active Publication Date: 2021-01-15
惠生(中国)投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, in the prior art, while using star-shaped polyamide to prepare high-fluidity parts, although certain mechanical strength is guaranteed, the analysis and conclusion of star-shaped polyamide The mechanical test indicators can be found: 1) After a certain degree of branched structure is introduced into the polymer, the toughness and impact strength of the material will decrease to varying degrees, such as Trouillet-Fonti, etc. using trifunctional etheramine As a branching agent, the notched impact strength of star-shaped PA66 products prepared with monobasic / dibasic carboxylic acids as molecular weight regulators decreased by 39%-57%, and the elongation at break decreased from 30% to 1.7-2%; Nijenhuis’ patent The elongation at break of PA6 decreased from 55% to 30% after adding 1.4% star branching agent 2,4,6-tris(aminocaproic acid)-1,3,5-triazine (TACT); 2) In addition, star-shaped polyamide itself has no chain winding, low crystallinity, and crystallization speed is significantly lower than that of linear polyamide. The decline in crystallization performance leads to extension of material injection molding cycle and reduces production efficiency

Method used

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  • Preparation method of long-chain star-shaped branching agent and high-fluidity high-crystallinity long-carbon-chain star-shaped polyamide
  • Preparation method of long-chain star-shaped branching agent and high-fluidity high-crystallinity long-carbon-chain star-shaped polyamide
  • Preparation method of long-chain star-shaped branching agent and high-fluidity high-crystallinity long-carbon-chain star-shaped polyamide

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preparation example Construction

[0048] The first aspect of the present invention provides a method for preparing a long-chain star-shaped branching agent. The two-step method can control the arm length and molecular weight of the prepared long-chain star-shaped branching agent. The preparation method of described long-chain star branching agent comprises the steps:

[0049] 1) reacting cyclohexanedicarboxylic acid chloride with long carbon chain diamine and the first acid-binding agent through interfacial polymerization to obtain a low molecular weight polymer;

[0050] 2) Continue reacting cyclohexanealkyl acid chloride with the low molecular weight polymer described in step 1) to prepare a long-chain star-shaped branching agent; wherein, the functionality of the cyclohexanealkyl acid chloride is more than or equal to 3.

[0051] The cyclohexane alkyl acid chloride is that cyclohexane is connected with alkyl acid chloride groups, and the number of alkyl acid chloride groups is more than or equal to 3. In o...

Embodiment 1

[0100] Add 500ml of toluene and 30g of triphosgene to the three-necked flask, keep stirring for 1h, transfer the three-necked flask to the ice-water mixing bath, slowly add 26g of 1,2,4,5-cyclohexanetetracarboxylic acid and 1ml of N,N-dimethyl Dimethicone formamide continued to react for 2h, transferred to an oil bath, continued to react at 50°C for 4h, and distilled under reduced pressure to obtain 1,2,4,5-cyclohexanetetracarbonyl chloride. 1,4-Cyclohexanedicarboxylic acid was used to prepare 1,4-cyclohexanedicarboxylic acid under the same conditions. Add 174.2g 1,4-cyclohexanediformyl chloride, 175.5g decanediamine, 550ml deionized water, 500ml toluene, 168g tetrabutylammonium hydroxide, continue stirring at 40°C for 30min, add 31.0g 1,2,4 , 5-cyclohexane tetracarbonyl chloride, stirred for 10min. Cool down, filter, and vacuum-dry to obtain the long-chain star branching agent S1.

[0101] 10 kg of sebacyl decanediamine salts were successively put into the autoclave, wherei...

Embodiment 2

[0103] Add 500ml of toluene and 15g of triphosgene to the three-necked flask, keep stirring for 1h, transfer the three-necked flask to an ice-water mixing bath, slowly add 13g of 1,2,4,5-cyclohexanetetracarboxylic acid and 0.5ml of N,N-di Methylformamide continued to react for 2h, transferred to an oil bath, continued to react at 50°C for 4h, and distilled under reduced pressure to obtain 1,2,4,5-cyclohexanetetracarbonyl chloride. In the same way, 1,4-cyclohexanedicarboxylic acid was used to obtain difunctional 1,4-cyclohexanediformyl chloride. Add 310g 1,4-cyclohexanedicarbonyl chloride, 287g decanediamine, 550ml deionized water, 500ml toluene, 116g urea, continue stirring at 70°C for 1h, then add 31g 1,2,4,5-cyclohexane Alkane tetracarbonyl chloride, stirred for 10 min to obtain long-chain star branching agent S2.

[0104]In the autoclave, drop into 10kg of sebacyl decanediamine salt successively, 490g long-chain star branching agent S2, 48g decanediamine, 97g benzoic acid,...

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Abstract

The invention relates to the field of star-shaped polyamide material preparation, in particular to a preparation method of a long-chain star-shaped branching agent and high-fluidity high-crystallinitylong-carbon-chain star-shaped polyamide. The preparation method of the long-chain star-shaped branching agent comprises the following steps: 1) carrying out interfacial polymerization reaction on cyclohexanedicarbonyl chloride, long-carbon-chain diamine and a first acid-binding agent to prepare a low-molecular-weight polymer; and 2) further reacting cyclohexanealkyl acyl chloride with the low-molecular-weight polymer obtained in the step 1) to prepare the long-chain star-shaped branching agent, wherein the functionality of the cyclohexane alkyl acyl chloride is greater than or equal to 3. Thelong-carbon-chain star polyamide prepared by reacting the long-chain star branching agent with a long-carbon-chain nylon salt, an assistant, water and the like has the advantages of high crystallization speed, favorable flowability, favorable impact resistance and the like.

Description

technical field [0001] The invention relates to the field of preparation of star-shaped polyamide materials, in particular to a long-chain star-shaped branching agent and a preparation method of high-fluidity and high-crystallization long-carbon-chain star-shaped polyamide. Background technique [0002] Star polyamide is a kind of branched polyamide with not less than three chains (arms), and the branches are all connected to the core in the form of chemical bonds. Compared with the traditional linear polyamide, the star polyamide has a certain three-dimensional network structure, which reduces the entanglement between the linear polyamide segments, and the shear thinning is more obvious in the molten state, which can Effectively reduce the viscosity of the melt during polyamide processing and increase its fluidity. It can usually be used as a modified material to increase the fluidity of glass fiber reinforced composite materials. When used as a heat-conducting material, mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/26C08G69/28
CPCC08G69/265C08G69/28
Inventor 王磊刘浩宇陈浩陈炫
Owner 惠生(中国)投资有限公司
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