CN102642902A

CN102642902A - Sewage flocculating agent preparation method

Info

Publication number: CN102642902A
Application number: CN2012101305012A
Authority: CN
Inventors: 贯硕磉; 杜宝燕; 陈芳
Original assignee: 廊坊格瑞泰化工有限公司
Priority date: 2012-04-28
Filing date: 2012-04-28
Publication date: 2012-08-22
Also published as: CN102642902B

Abstract

The invention discloses a sewage flocculating agent preparation method. The method includes: adding 2-straightchain alkylamine into mixed liquid of 1-halogen-2,3-epoxypropane with water under the inert gas shielding and under the temperature of T1=0-50 DEG C; heating to the temperature of T2=70-100 DEG C for reaction until pH (potential of hydrogen) of the reaction liquid is equal to or smaller than 7.0; cooling the reaction liquid, adding post-treating agent for treatment, and adjusting the reaction liquid to be neutral to obtain the flocculating agent. The method has the advantages of environment friendliness and simple process due to avoidance of high pressure, high temperature, waste gas, waste water and industrial residue. The flocculating agent obtained by the method has excellent degradability, low ecotoxicity and no stimulation to human body, has evident excellent flocculating effect on treatment of various complex wastewaters, embodies high cost performance in sludge dewatering, and has the advantages of harmlessness to human bodies, remnant avoidance, effectiveness in flocculating and wide application range.

Description

A kind of preparation method of sewage flocculant

Technical field

The present invention relates to a kind of preparation method of water conditioner, especially a kind of preparation method of sewage flocculant.

Background technology

World's water pollution problems is on the rise at present, and it is more and more severeer that water treatment problems also becomes.Be to solve water pollution problems, adopt the flocculation agent precipitator method as a kind of lower-cost water treatment method by extensive employing.Flocculation is to the important process in water security purification and the wastewater treatment, and flocculation agent directly influences flocculating effect.Flocculation agent is mainly used in sewage treatment area, can reduce the sense index such as turbidity, colourity of former water, removes multiple macromolecule organic, heavy metal and radioactive substance.Flocculation both can have independently treatment system of one's own, also can make up with other processing unit process, as pre-treatment, intermediate treatment and final treating processes, also can be used for the preceding concentration process of sludge dewatering, improved the dewatering of mud.

Generally use at present aluminium salt, SEPIGEL 305 flocculation agent as water.These two types of flocculation agents effect in application is general, and especially effect is bad in sewage or complicated sewage, can not adapt to modern industry and development of city; And they have human body stimulates and degradation property is poor, residual quantity is big in the water, can cause secondary pollution.

Summary of the invention

The technical problem that the present invention will solve provides a kind of effective, toxicological harmless, is prone to the preparation method of the sewage flocculant of degraded.

For solving the problems of the technologies described above, the technical scheme that the present invention taked is: at T ₁Under=0～50 ℃, protection of inert gas, two straight chain alkyl amines are added to 1-halogen-2, in the mixed solution of 3-propylene oxide and water; Be warming up to T then ₂=70～100 ℃ of reactions are to pH≤7.0 of reaction solution; With the reaction solution cooling, add post-treatment agent then and handle, again reaction solution is transferred to neutrality, promptly obtain described flocculation agent.

Two straight chained alkyls according to the invention and 1-halogen-2, the mol ratio of 3-propylene oxide are 1.2:1～1:1.2.

Preferred two straight chain alkyl amines of the present invention are n n dimetylaniline or diethylamine; Preferred 1-halogen-2, the 3-propylene oxide is epoxy chloropropane or 1-bromo-2, the 3-propylene oxide.

Rare gas element of the present invention is nitrogen or carbonic acid gas.

Post-treatment agent of the present invention is selected from S-WAT, ydrogen peroxide 50, sodium hydroxide, Sulfothiorine or POTASSIUM BOROHYDRIDE 97MIN.The add-on of said post-treatment agent is 0.01%～1% of a reaction solution total mass.

The preferred T of the present invention ₁It is 10～30 ℃; Preferred T ₂It is 80～90 ℃.

Preferred reaction liquid of the present invention react to pH be 6.0～7.0.

Reaction solution according to the invention is cooled to 0～70 ℃; Preferably be cooled to 30～60 ℃.

The resultant flocculation agent of the present invention has following general formula ():

In the formula ():

R1: be selected from H, by a kind of saturated or undersaturated alkyl that has at least one carbon atom;

R2: be selected from H, by a kind of saturated or undersaturated alkyl that has at least one carbon atom;

N is 1～100000;

X: represent a kind of halide-ions that combines with positively charged ion, preferably be selected from chlorine, bromine.

Adopt the beneficial effect that technique scheme produced to be: the inventive method does not have high pressure, no high temperature, and does not have any three wastes generation, therefore has environmental protection, technology characteristic of simple.The flocculation agent that the present invention obtains has good degradation property, eco-toxicity low, non-stimulated to human body, and to handling various complex wastewaters significantly good flocculating effect is arranged, and the dehydration of mud is embodied good cost performance; Have human non-toxic evil, noresidue, good, the advantage of wide range of application of flocculating effect.

Embodiment

Below in conjunction with specific embodiment the present invention is done further detailed explanation.

Embodiment 1: the preparation method of this sewage flocculant adopts following process step.

In reactor drum, add 200g deionized water, 4.39mol epoxy chloropropane, less than 100ppm, open stirring, be cooled to 10 ℃, begin to drip the 40wt% aqueous solution of n n dimetylaniline (4.39mol) with nitrogen replacement to oxygen level; After dripping off, n n dimetylaniline is warming up to 80 ℃, constant temperature 10 hours, and sampling monitoring pH value to pH=6.5, is cooled to 60 ℃, adds the S-WAT of reaction solution quality 0.5%, stirs 2 hours, regulates pH to neutral with sodium hydroxide again, has both got finished product.

Embodiment 2: the preparation method of this sewage flocculant adopts following process step.

In reactor drum, add 400g deionized water, 4.4mol epoxy chloropropane, less than 100ppm, open stirring, be cooled to 30 ℃, begin to drip diethylamine (4.38mol) with nitrogen replacement to oxygen level; After dripping off, diethylamine is warming up to 70 ℃, constant temperature 10 hours, and sampling monitoring pH value is to pH=6.0; Be cooled to 30 ℃, add the Sulfothiorine of reaction solution quality 1.0%, stirred 1 hour, regulate pH to neutral with Pottasium Hydroxide again, both got finished product.

Embodiment 3: the preparation method of this sewage flocculant adopts following process step.

In reactor drum, add 200g deionized water, 4.38mol1-bromo-2, the 3-propylene oxide less than 100ppm, is opened stirring with carbon dioxide replacement to oxygen level, is cooled to 50 ℃, begins to drip n n dimetylaniline (4.4mol) aqueous solution; After dripping off, n n dimetylaniline is warming up to 90 ℃, constant temperature 10 hours, and sampling monitoring pH value is to pH=7.0; Be cooled to 0 ℃, add the ydrogen peroxide 50 of reaction solution quality 0.1%, stirred 3 hours, regulate pH to neutral with sodium hydroxide again, both got finished product.

Embodiment 4: the preparation method of this sewage flocculant adopts following process step.

In reactor drum, add 600g deionized water, 4.8mol1-bromo-2, the 3-propylene oxide less than 100ppm, is opened stirring with nitrogen replacement to oxygen level, is cooled to 0 ℃, begins to drip diethylamine (4.00mol); After dripping off, diethylamine is warming up to 100 ℃, constant temperature 5 hours, and sampling monitoring pH value is to pH=6.8; Be cooled to 70 ℃, add the POTASSIUM BOROHYDRIDE 97MIN of reaction solution quality 0.2%, stirred 2.5 hours, regulate pH to neutral with Pottasium Hydroxide again, both got finished product.

Embodiment 5: the preparation method of this sewage flocculant adopts following process step.

In reactor drum, add 600g deionized water, 4.00mol epoxy chloropropane, less than 100ppm, open stirring, be cooled to 20 ℃, begin to drip diethylamine (4.8mol) with carbon dioxide replacement to oxygen level; After dripping off, diethylamine is warming up to 85 ℃, constant temperature 20 hours, and sampling monitoring pH value is to pH=6.8; Be cooled to 45 ℃, add the sodium hydroxide of reaction solution quality 0.01%, stirred 1.5 hours, regulate pH to neutral with sodium hydroxide again, both got finished product.

Claims

1. the preparation method of a sewage flocculant is characterized in that: at T ₁Under=0～50 ℃, protection of inert gas, two straight chain alkyl amines are added to 1-halogen-2, in the mixed solution of 3-propylene oxide and water; Be warming up to T then ₂=70～100 ℃ of reactions are to pH≤7.0 of reaction solution; With the reaction solution cooling, add post-treatment agent then and handle, again reaction solution is transferred to neutrality, promptly obtain described flocculation agent.

2. the preparation method of a kind of sewage flocculant according to claim 1, it is characterized in that: said two straight chained alkyls and 1-halogen-2, the mol ratio of 3-propylene oxide are 1.2:1～1:1.2.

3. the preparation method of a kind of sewage flocculant according to claim 1, it is characterized in that: described two straight chain alkyl amines are n n dimetylaniline or diethylamine; Described 1-halogen-2,3-propylene oxide are epoxy chloropropane or 1-bromo-2, the 3-propylene oxide.

4. the preparation method of a kind of sewage flocculant according to claim 1, it is characterized in that: described rare gas element is nitrogen or carbonic acid gas.

5. the preparation method of a kind of sewage flocculant according to claim 1, it is characterized in that: described post-treatment agent is selected from S-WAT, ydrogen peroxide 50, sodium hydroxide, Sulfothiorine or POTASSIUM BOROHYDRIDE 97MIN.

6. the preparation method of a kind of sewage flocculant according to claim 5, it is characterized in that: the add-on of said post-treatment agent is 0.01%～1% of a reaction solution total mass.

7. according to the preparation method of described any one sewage flocculant of claim 1-6, it is characterized in that: said T ₁It is 10～30 ℃; Said T ₂It is 80～90 ℃.

8. according to the preparation method of described any one sewage flocculant of claim 1-6, it is characterized in that: said reaction solution react to pH be 6.0～7.0.

9. according to the preparation method of described any one sewage flocculant of claim 1-6, it is characterized in that: said reaction solution is cooled to 0～70 ℃.

10. the preparation method of a kind of sewage flocculant according to claim 9, it is characterized in that: said reaction solution is cooled to 30～60 ℃.