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Preparation method of poly dimethyl allyl ammonium chloride with high relative molecular mass

A technology of dimethyl diallyl ammonium chloride and relative molecular weight, which is applied in the field of preparation of cationic water-soluble polymers, can solve the problem of not being able to point out the type of impurities and their content, difficult to obtain reliable results, and low degree of industrialization and other problems, to achieve the effect of high relative molecular weight of the product, good economy and applicability, and lower activation energy

Active Publication Date: 2007-12-05
NANJING UNIV OF SCI & TECH
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  • Abstract
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  • Claims
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Problems solved by technology

However, the former has the problems of poor industrialization and high prices, while the latter has problems of storage stability (documents 1, 2, 3)
[0014] (2) The method of continuously dropping the initiator at a high temperature of 105-115°C, or the method of from 40°C to 60°C, and then from 60°C to 40°C for a period of more than 72 hours, the polymerization reaction is relatively Harsh and complex, low degree of industrialization (References 3, 4)
[0015] (3) All the methods for preparing PDMDAAC so far cannot point out the type of impurities and their content in the raw material monomers that have the most direct impact on the relative molecular weight of the product
This problem also exists even with the use of poorly industrialized two-step monomers
As a result, due to the different preparation methods of the monomer, or the different batches of the same method, as a result, the impurity content is different, resulting in poor stability of the preparation process
Therefore, the existing methods reported in the literature are often difficult to obtain reliable results

Method used

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  • Preparation method of poly dimethyl allyl ammonium chloride with high relative molecular mass
  • Preparation method of poly dimethyl allyl ammonium chloride with high relative molecular mass

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: in conjunction with accompanying drawing, the specific embodiment of the preparation method of high relative molecular mass polydimethyldiallyl ammonium chloride is:

[0036] In the first step, the refined one-step industrial monomer DMDAAC solution with a mass fraction of 60% is used, and the main impurities contained in it are less than 1 mg / kg of allyl chloride, dimethylamine, allyl aldehyde, and allyl alcohol. Dimethylamine (tertiary amine) amount 19mg / kg, dimethylamine hydrochloride 700mg / kg, allyl dimethylamine hydrochloride (tertiary amine salt) 500mg / kg; sodium chloride amount 2000mg / kg, The amount of Fe and Cu ions is less than 1mg / kg. In the reactor, 33.5±0.5kg of monomer DMDAAC was heated and distilled under reduced pressure, and dehydrated to a mass fraction of 83.1%.

[0037] In the second step, add 100g of ammonium persulfate and Na 4 1.0 kg of aqueous solution of 2.0 g of EDTA, which accounts for about 0.35% and 0.0071% of the mass of the ...

Embodiment 2-5

[0041] Embodiment 2-5: in conjunction with accompanying drawing, process condition is the same as embodiment 1, is different from the substance content of embodiment 1, and its product performance result is listed in comparison table 1. Wherein MPS, APS, PPS and SPS are persulfate, ammonium persulfate, potassium persulfate and sodium persulfate respectively.

[0042] Table 1 Comparison of the preparation results of Examples 1-5

[0043] Preface

No

Raw material monomer (after dehydration)

Initiator dosage (accounting for monomer mass fraction, grams)

starting monomer

Content / %

product

PDMDAAC

[η] / dL / g

monomer conversion

/ %

Monomer content / %

Mass / kg

MPS / %(g)

Na 4 EDTA / %(g)

Example

1

83.1

33.5

(APS, ammonium salt)

0.35 (97.4)

0.0071(2.00)

65.0

3.99

99.0

Ex...

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Abstract

The present invention discloses preparation process of polyammonium dimethyldiallyl chloride with relatively high molecular weight. By using ammonium dimethyldiallyl chloride with high purity as material, and through adding initiator and complexing agent at certain temperature and stepped temperature raising for slow releasing of the initiator and stepped initiation of the polymerization, colloidal or powdered polyammonium dimethyldiallyl chloride is prepared. The process has high technological stability, low production cost and easy operation, and the product has relatively high molecular weight and various uses.

Description

technical field [0001] The invention belongs to the preparation technology of cationic water-soluble polymers, in particular to a preparation method of high relative molecular weight polydimethyldiallylammonium chloride. Background technique [0002] Poly-dimethyldiallyl ammonium chloride (PDMDAAC for short) is a water-soluble polymer compound with a cationic quaternary ammonium salt group. Dimethyldiallyl ammonium chloride (DMDAAC for short) is obtained through free radical polymerization, and its molecular structure and preparation reaction formula are as follows: [0003] [0004] In the formula, n=2, 3, 4, ... n; m = 2, 3, 4, ... m. [0005] PDMDAAC is white water-absorbing powder, soluble in water, methanol and glacial acetic acid, insoluble in other solvents. Its products are generally aqueous solutions, but there are also dry powder products. At room temperature, PDMDAAC aqueous solution is stable in the pH range of 0.5-14. Due to good water solubility, high po...

Claims

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Application Information

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IPC IPC(8): C08F136/02C08F4/30
CPCC08F226/04
Inventor 张跃军贾旭
Owner NANJING UNIV OF SCI & TECH
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