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Preparation method of VP/alpha-olefin copolymer and VP/alpha-olefin copolymer

An olefin copolymer and olefin technology, which is applied in the preparation of VP/α-olefin copolymers, and the field of VP/α-olefin copolymers, can solve the problem of increasing the content of cross-linked gelling impurities, production costs, product application limitations, and restrictions on copolymerization. Product production efficiency and other issues, to achieve high reaction efficiency, avoid cross-linking gel and chain scission, and achieve uniform and controllable copolymerization reactions

Active Publication Date: 2017-10-10
SHANGHAI YUKING WATER SOLUBLE MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the reaction rate of the copolymerization reaction of this technical scheme is low, needs higher reaction temperature and very long reaction time, causes the energy consumption of copolymerization reaction big,, production cost is high, has directly restricted the production efficiency of copolymerization product; Excessive production The cost also leads to great restrictions on the application of the product
In addition, side reactions are obvious at higher reaction temperatures, such as: cross-linked gelation of PVP, chain scission at high temperature, and increased impurity content, etc., which increases the complexity of product purification, further increases production costs, and limits its industry. application

Method used

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  • Preparation method of VP/alpha-olefin copolymer and VP/alpha-olefin copolymer
  • Preparation method of VP/alpha-olefin copolymer and VP/alpha-olefin copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] The preparation of embodiment 1, VP / α-olefin copolymer

[0055] (1), α-olefin preactivation

[0056] Mix 3.59g of dodecene and 3.59g of ethanol evenly, add 0.0718g of triisobutylaluminum for preactivation, and obtain mixture A for subsequent copolymerization; the preactivation temperature is controlled at 10°C, and the preactivation time is 30 minutes , The pre-activation process is a reflux process under the protection of nitrogen.

[0057] (2), pre-copolymerization reaction

[0058] Add 10g of PVPK15, 0.19g of dodecene, 0.027g of benzoyl peroxide, 0.041g of tert-butyl peroxide, 0.0068g of ascorbic acid, and 100g of ethanol into a four-necked flask with a stirring and condensing device, and stir until completely dissolved Afterwards, nitrogen gas was introduced for replacement, and then the pre-copolymerization reaction was carried out at 40°C. The pre-copolymerization reaction was a reflux reaction, and the pre-copolymerization reaction time was controlled to be 30 ...

Embodiment 2

[0063] The product VP / α-olefin copolymer is a white solid, insoluble in water, and has good solubility in hydrocarbon solvents. Detect residual single and residual initiator in the product respectively, as shown in Table 2. After calculation, the grafting rate of monomer olefin is 100%. The preparation of embodiment 2, VP / α-olefin copolymer

[0064] (1), α-olefin preactivation

[0065] Mix 151.3g of hexadecene and 90.5g of isopropanol evenly, add 6.44g of triethylaluminum for preactivation, and obtain mixture A for subsequent copolymerization; the preactivation temperature is controlled at 15°C, and the preactivation time is 40 Minutes, the pre-activation process is a reflux process under the protection of nitrogen.

[0066] (2), pre-copolymerization reaction

[0067] Add 20g of PVPK30, 9.66g of hexadecene, 4.24g of diacetyl peroxide, 10.49g of di-tert-butyl peroxide, 2.946g of ascorbic acid, and 100g of isopropanol into a four-necked flask with a stirring and condensing d...

Embodiment 3

[0073] The preparation of embodiment 3, VP / α-olefin copolymer

[0074] (1), α-olefin preactivation

[0075] Mix 52.2g of hexene and 26.1g of 3-methyl-1-butanol evenly, add 2.838g of diethylaluminum chloride for preactivation, and obtain mixture A for subsequent copolymerization; the preactivation temperature is controlled at 25 °C, the pre-activation time is 50 minutes, and the pre-activation process is a reflux process under the protection of nitrogen.

[0076] (2), pre-copolymerization reaction

[0077] Add 25g PVPK90, 4.54g hexene, 5.41g tert-butyl peroxyisobutyrate, 9.13g dicumyl peroxide, 4.36g BHT, 100g 3-methyl-1-butanol respectively into the In the four-necked flask of the device, stir until the dissolution is complete, pass nitrogen replacement protection, and then control the pre-copolymerization reaction at 90 ° C, the pre-copolymerization reaction is a reflux reaction, and the time of the pre-copolymerization reaction is controlled for 40 minutes to obtain a pre-...

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Abstract

The invention discloses a preparation method of a VP / alpha-olefin copolymer. The method comprises the following steps: (1), pre-activating a part of alpha-olefin to obtain a mixture A; (2), pre-copolymerization reaction: carrying out pre-copolymerization reaction on PVP (polyvinylpyrrolidone), the remaining alpha-olefin in the step (1), a compound initiating agent, an activating agent and an organic solvent at a controlled temperature of 40 to 90 DEG C to obtain a pre-copolymerized mixture B; (3), copolymerization reaction: adding the mixture A into the pre-copolymerized mixture B and controlling total reaction time of the step (2) and the step (3) to be 4 to 10 hours to obtain a copolymerized mixture C; (4), carrying out product separation on the copolymerized mixture C to obtain the VP / alpha-olefin copolymer. According to the preparation method of the VP / alpha-olefin copolymer, the temperature and the reaction time required by the copolymerization reaction can be effectively reduced, a reaction condition is mild, the reaction is easily controlled, the purity of the product is high, and complicated purification treatment on the product is not needed, so that the production efficiency is effectively improved, the production cost is reduced, and extended application of the VP / alpha-olefin copolymer is facilitated.

Description

technical field [0001] The invention belongs to the technical field of polymer polymerization, and in particular relates to a preparation method of a VP / α-olefin copolymer and the VP / α-olefin copolymer. Background technique [0002] The molecular structure of N-vinylpyrrolidone (NVP) monomer contains vinyl structure, which is very easy to undergo polymerization reaction. N-vinylpyrrolidone monomer can not only undergo copolymerization reaction with other unsaturated monomers containing vinyl structure to form copolymers, but also undergo homopolymerization reaction itself to form polyvinylpyrrolidone (PVP). PVP has good water solubility, and its solubility in water is only limited by its own viscosity. It also has good solubility in some organic solvents (such as methanol, ethanol, ether-alcohols, amines, etc.), but it is in most fats. Insoluble in hydrocarbon organic solvents (such as hexane, heptane, cyclohexane, methylcyclohexane, mineral oil, lubricating oil and some no...

Claims

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Application Information

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IPC IPC(8): C08F271/02C08F210/14
CPCC08F271/02C08F210/14
Inventor 王宇朱广东陈占熊俊超
Owner SHANGHAI YUKING WATER SOLUBLE MATERIAL TECH
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