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Method for preparing dimethyldiallyl ammonium chloride and sulfur dioxide co-polymer PAS

A technology of dimethyl diallyl ammonium chloride and sulfur dioxide is applied in the field of preparation of dimethyl diallyl ammonium chloride and sulfur dioxide copolymer PAS, which can solve the difficulty of increasing storage and transportation, and cannot guarantee the preparation of It can achieve the effect of good industrialization foundation, low production cost and easy operation.

Active Publication Date: 2010-12-15
武汉松石科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] (1) The DMDAAC used in documents 1, 2, and 3 are all solids, and organic solvents are used in the production process to greatly reduce the economy of the PAS preparation process
[0012] (2) The PAS synthesized in Documents 1, 2, and 3 are all solid in the end, and organic solvents are used for crystallization, which is not conducive to clean production
And the PAS solid is extremely easy to absorb moisture, which increases the difficulty of storage and transportation
[0013] (3) In Documents 1 and 3, SO 2 Soluble in organic solvents, which is not conducive to industrial production
[0014] (4) In document 2, add SO in batches 2 , the ratio of the two monomers cannot be guaranteed to be stable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1: the preparation method of PAS of the present invention, comprises the following steps:

[0045] The first step: add 361Kg industrial grade DMDAAC aqueous solution (mass fraction is 45%) in reactor, when -10~-5 ℃, pass into N under stirring 2 For 10 minutes, the flow rate was 100 L / h, and the air in the reaction system was removed.

[0046] The second step: at the temperature of -10 ~ -5 ° C, under stirring, pass SO 2 , the access time is 4h, and the input volume is 63.5Kg.

[0047] The third step: when the temperature is -10~-5℃, add 162g Na 4 EDTA.

[0048] Step 4: Slowly add 9 Kg of ammonium persulfate aqueous solution (content: 12%) under stirring at a temperature of -10 to -5° C., and the dropping time is 0.5 to 1 hour. At the temperature of -10~-5°C, under stirring, keep the reaction for 1h.

[0049] Step 5: Under stirring, raise the temperature of the reaction solution to 30-35° C., slowly add 18 Kg of ammonium persulfate aqueous solution (conte...

Embodiment 2

[0053] Embodiment 2: the preparation method of PAS of the present invention comprises the following steps:

[0054] The first step: add 250Kg industrial grade DMDAAC aqueous solution (mass fraction is 65%) in reactor; When -10~-5 ℃, pass into N under stirring 2 For 10 minutes, the flow rate was 100 L / h, and the air in the reaction system was removed.

[0055] The second step: at the temperature of -10 ~ -5 ° C, under stirring, pass SO 2 , the access time is 4h, and the input volume is 63.5Kg.

[0056] The third step: when the temperature is -10~-5℃, add 162g Na 4 EDTA.

[0057] Step 4: Slowly add 9Kg of ammonium persulfate aqueous solution (12% content) under stirring at a temperature of -10~-5°C, and dropwise adding time is 0.5~1h; at a temperature of -10~-5°C , Under stirring, heat preservation reaction 1h.

[0058] Step 5: Under stirring, raise the temperature of the reaction solution to 30-35° C., slowly add 18 Kg of ammonium persulfate aqueous solution (content: 12%)...

Embodiment 3

[0062] Embodiment 3: the preparation method of PAS of the present invention, comprises the following steps:

[0063] The first step: add 295Kg industrial grade DMDAAC aqueous solution (mass fraction is about 55%) in the reactor; 2 For 10 minutes, the flow rate was 100 L / h, and the air in the reaction system was removed.

[0064] The second step: when the temperature is -5 ~ 0 ° C, under stirring, pass SO 2 , the access time is 4h, and the input volume is 63.5Kg.

[0065] Step 3: Add 162g Na 4 EDTA.

[0066] Step 4: Slowly add 9Kg of ammonium persulfate aqueous solution (12% content) under stirring at a temperature of -5 to 0°C, dropwise for 0.5 to 1 hour; keep the temperature at -5 to 0°C and stir Next, keep warm for 1h.

[0067] Step 5: Under stirring, raise the temperature of the reaction solution to 30-35°C, slowly add 18Kg of ammonium persulfate aqueous solution (content: 12%), dropwise for 1.5-2 hours; keep the temperature at 30-35°C, and stir Next, keep warm for 1h...

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PUM

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Abstract

The invention discloses a method for preparing a copolymer PAS of dimethyl diallyl ammonium chloride and sulfur dioxide. The method comprises the following steps: using industrial cationic monomer dimethyl diallyl ammonium chloride aqueous solution as a raw material; introducing industrial-grade sulfur dioxide into the raw material, then adding Na4EDTA once as a complexing agent; gradually and slowly adding peroxide as an initiator; controlling the reaction temperature while stirring; controlling the reaction rate according to gradient temperature raising; initiating the polyreaction of the dimethyl diallyl ammonium chloride and the sulfur dioxide at lower temperature to increase the polymerization degree of PAS products and improve the relative molecular weight; adding the residual initiator at higher temperature in the final stage of reaction in order to improve the conversion rate of the monomer in the product; and finally controlling the quantity of the added dilution water to regulate the solid content of the product. The method has good economic benefit and industrial foundation; and because the trigger temperature is moderate and the polymerization is performed under the milder condition, the operation is easy and the production cost is low.

Description

technical field [0001] The invention relates to a preparation method of dimethyl diallyl ammonium chloride and sulfur dioxide copolymer PAS, which belongs to the industrial preparation technology of cationic quaternary ammonium salt and sulfur dioxide copolymer. Background technique [0002] PAS (polysulfone) is a cationic quaternary ammonium salt monomer, the copolymerization product of dimethyl diallyl ammonium chloride (DMDAAC for short) and sulfur dioxide. PAS is an aqueous linear polymer with cationic quaternary ammonium salt groups, and it is also a cationic polyelectrolyte. PAS is white water-absorbing powder, easily soluble in water, insoluble in organic solvents. [0003] Currently commercially available products are aqueous solutions, and PAS aqueous solutions are stable in the range of pH<6.5 at room temperature. Due to its non-toxicity, good water solubility, and high positive charge density, PAS can be widely used in fields such as petroleum exploration, pa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/22
Inventor 周烈平陈立霞魏良义陈曦刘义津余红华
Owner 武汉松石科技股份有限公司
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