CN103881090A - Production technology for high-molecular cation flocculating agent - Google Patents

Production technology for high-molecular cation flocculating agent Download PDF

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Publication number
CN103881090A
CN103881090A CN201210553352.0A CN201210553352A CN103881090A CN 103881090 A CN103881090 A CN 103881090A CN 201210553352 A CN201210553352 A CN 201210553352A CN 103881090 A CN103881090 A CN 103881090A
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China
Prior art keywords
solution
azacyclopropane
ethyleneimine
generate
parts
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CN201210553352.0A
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Chinese (zh)
Inventor
张述智
夏伟
朱绍辉
张�浩
王晓丽
徐权汗
李之详
许团辉
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Qingdao Zhongren Pharmaceutical Coltd
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Qingdao Zhongren Pharmaceutical Coltd
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Priority to CN201210553352.0A priority Critical patent/CN103881090A/en
Publication of CN103881090A publication Critical patent/CN103881090A/en
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Abstract

A disclosed production technology for a high-molecular cation flocculating agent comprises: reacting ethanolamine with hydrogen chloride gas in a spray absorption tower to generate ethanolamine hydrochloride; enabling ethanolamine hydrochloride to enter a fluidized bed reaction tower, under 20 DEG C, reacting with thionyl chloride; sending the products to a decomposition tank, so as to decompose the products under the condition of strong heat of 30 DEG C or more and release sulfur dichloride and chloroethylamine hydrochloride; adding sodium hydroxide into chloroethylamine hydrochloride, stirring for 1 h with cooling, so as to obtain an alkaline ethyleneimine solution; enabling the alkaline ethyleneimine solution to enter a distillation still for distillation and distilling out ethyleneimine; enabling ethyleneimine to enter a polymerization kettle, adding water and hydrochloric acid, introducing a proper amount of carbon dioxide, so as to perform a ring-opening polymerization reaction on the ethyleneimine solution and generate an aqueous solution of polyethylenimine; and after the polymerization reaction is finished, adjusting the pH value to 10 with sodium hydroxide, so as to obtain a finished product. The produced high-molecular cation flocculating agent is wide is applicable pH value scope (with best effect when pH is 4-10), can generate good effect both with a high concentration and at a low temperature, and is less in usage amount and low in price.

Description

The production technique of macromolecule cation flocculation agent
 
Technical field
The invention belongs to flocculation agent production technical field, be specifically related to the production technique of macromolecule cation flocculation agent.
 
Background technology
Flocculent precipitation is to select inorganic flocculating agent (as Tai-Ace S 150) and organic anion type flocculation agent Polyacrylamide (PAM) to be mixed with the aqueous solution to add in waste water, just can produce compression double electric layer, make the suspended particulates loss of stability in waste water, the mutual coagulation of micelle thing phase increases particulate, forms flocs unit, alumen ustum.Flocs unit is grown up and under action of gravity, depart from aqueous phase precipitation after certain volume, thereby removes a large amount of suspended substances in waste water, thereby reaches the effect of water treatment.For improving separating effect, can add in good time, in right amount coagulant aids.Sewage after treatment be in colourity, substantially can reach emission standard containing aspects such as chromium, suspension content, can beyond row or the re-injection water that recovers the oil as man-made injection.
Cation polymeric flocculant has good flocculating effect to waste water from dyestuff.Positive ion organic high polymer coagulant kind is relatively less, the sixties in 20th century, first Schuller etc. have reported the method for acrylamide and the copolymerization simultaneously of the dimethyl diallyl ammonium chloride aqueous solution, and positive ion organic high polymer coagulant raised path between farm fields makes flocculation agent be adsorbed in electronegative suspended particle, electronegative emulsified oil droplet and be contained in the water-soluble organic colloid of anionic group by electrostatic interaction.In and microparticle surfaces electric charge make its cohesion unstability in the situation that, can further utilize the adsorption bridging effect of its long molecular chain, make suspended particle cohesion, flocculating settling, that emulsified oil droplet cohesion becomes is large, floating or breakdown of emulsion, therefore it has the dual-use function of cohesion and flocculation, is a kind of multifunctional flocculants.But macromolecule cation flocculation agent prepared by existing technique exists applicable pH range narrower more, to the water treatment poor effect of high density and low temperature, consumption is many, expensive defect.
 
Summary of the invention
The above-mentioned defect existing in order to overcome prior art field, the object of the invention is to, a kind of production technique of macromolecule cation flocculation agent is provided, macromolecule cation flocculation agent prepared by solution prior art exists applicable pH range narrower more, to the water treatment poor effect of high density and low temperature, consumption is many, expensive defect.
The production technique of macromolecule cation flocculation agent provided by the invention, comprises the following steps:
(1) by 710 parts of thanomins in spray absorber tower with 425 parts of hydrogen chloride gas precursor reactants, generate ethanolamine hydrochloric salt, the reaction gas of generation is taken away by recirculation cooler;
(2) ethanolamine hydrochloric salt enters as fluid bed reacting tower, below 20 ℃, reacts with 1384 parts of sulfur oxychlorides, and the hydrogen chloride gas of generation imports spray absorber tower and recycles;
(3) product is delivered to and decomposed in cylinder, more than 30 ℃, after heat-flash, decompose, emit sulfur dichloride and chloroethylamine hydrochloride, sulfurous gas imports absorption tower and reclaims;
(4) chloroethylamine hydrochloride is added to 980 parts of sodium hydroxide, solution, cooling lower stirring 1 hour, obtains alkaline azacyclopropane solution;
(5) alkaline azacyclopropane solution enters still kettle distillation, steams azacyclopropane;
(6) azacyclopropane enters in polymeric kettle, adds water, hydrochloric acid, and pass into adaptation carbonic acid gas, azacyclopropane solution generation ring-opening polymerization and generate polyethyleneimine: amine aqueous solution, after polyreaction completes, with sodium hydroxide adjust pH be 10, be finished product;
The purity of described thanomin is greater than 98%.
The production technique of macromolecule cation flocculation agent provided by the invention, its beneficial effect is, applicable pH value wide (between pH4-10, effect is best), to high density, low temperature all has good effect, and consumption is few, cheap.
 
Embodiment
Below in conjunction with an embodiment, the production technique of macromolecule cation flocculation agent provided by the invention is described in detail.
 
Embodiment
The production technique of the macromolecule cation flocculation agent of the present embodiment, comprises the following steps:
(1) 710 parts of purity are greater than 98% thanomin in spray absorber tower with 425 parts of hydrogen chloride gas precursor reactants, generate ethanolamine hydrochloric salt, the reaction gas of generation is taken away by recirculation cooler;
(2) ethanolamine hydrochloric salt enters as fluid bed reacting tower, below 20 ℃, reacts with 1384 parts of sulfur oxychlorides, and the hydrogen chloride gas of generation imports spray absorber tower and recycles;
(3) product is delivered to and decomposed in cylinder, more than 30 ℃, after heat-flash, decompose, emit sulfur dichloride and chloroethylamine hydrochloride, sulfurous gas imports absorption tower and reclaims;
(4) chloroethylamine hydrochloride is added to 980 parts of sodium hydroxide, solution, cooling lower stirring 1 hour, obtains alkaline azacyclopropane solution;
(5) alkaline azacyclopropane solution enters still kettle distillation, steams azacyclopropane;
(6) azacyclopropane enters in polymeric kettle, adds water, hydrochloric acid, and pass into adaptation carbonic acid gas, azacyclopropane solution generation ring-opening polymerization and generate polyethyleneimine: amine aqueous solution, after polyreaction completes, with sodium hydroxide adjust pH be 10, be finished product.

Claims (2)

1. a production technique for macromolecule cation flocculation agent, is characterized in that: comprise the following steps:
(1) by 710 parts of thanomins in spray absorber tower with 425 parts of hydrogen chloride gas precursor reactants, generate ethanolamine hydrochloric salt, the reaction gas of generation is taken away by recirculation cooler;
(2) ethanolamine hydrochloric salt enters as fluid bed reacting tower, below 20 ℃, reacts with 1384 parts of sulfur oxychlorides, and the hydrogen chloride gas of generation imports spray absorber tower and recycles;
(3) product is delivered to and decomposed in cylinder, more than 30 ℃, after heat-flash, decompose, emit sulfur dichloride and chloroethylamine hydrochloride, sulfurous gas imports absorption tower and reclaims;
(4) chloroethylamine hydrochloride is added to 980 parts of sodium hydroxide, solution, cooling lower stirring 1 hour, obtains alkaline azacyclopropane solution;
(5) alkaline azacyclopropane solution enters still kettle distillation, steams azacyclopropane;
(6) azacyclopropane enters in polymeric kettle, adds water, hydrochloric acid, and pass into adaptation carbonic acid gas, azacyclopropane solution generation ring-opening polymerization and generate polyethyleneimine: amine aqueous solution, after polyreaction completes, with sodium hydroxide adjust pH be 10, be finished product.
2. the production technique of macromolecule cation flocculation agent according to claim 1, is characterized in that: the purity of described thanomin is greater than 98%.
CN201210553352.0A 2012-12-19 2012-12-19 Production technology for high-molecular cation flocculating agent Pending CN103881090A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210553352.0A CN103881090A (en) 2012-12-19 2012-12-19 Production technology for high-molecular cation flocculating agent

Publications (1)

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CN103881090A true CN103881090A (en) 2014-06-25

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104829782A (en) * 2015-05-12 2015-08-12 苏州市湘园特种精细化工有限公司 Preparation method of polymeric flocculant
CN108003036A (en) * 2017-12-29 2018-05-08 山东泰和水处理科技股份有限公司 A kind of preparation method of 2-chloroethyl amine hydrochloride
CN114479069A (en) * 2022-03-04 2022-05-13 四川大学 Novel method for directly synthesizing branched polyethyleneimine from haloethylamine

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104829782A (en) * 2015-05-12 2015-08-12 苏州市湘园特种精细化工有限公司 Preparation method of polymeric flocculant
CN108003036A (en) * 2017-12-29 2018-05-08 山东泰和水处理科技股份有限公司 A kind of preparation method of 2-chloroethyl amine hydrochloride
CN114479069A (en) * 2022-03-04 2022-05-13 四川大学 Novel method for directly synthesizing branched polyethyleneimine from haloethylamine

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Application publication date: 20140625