CN104987437A - Chlorinated polyethylene produced by one-step method and preparation method of chlorinated polyethylene - Google Patents
Chlorinated polyethylene produced by one-step method and preparation method of chlorinated polyethylene Download PDFInfo
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- CN104987437A CN104987437A CN201510428586.6A CN201510428586A CN104987437A CN 104987437 A CN104987437 A CN 104987437A CN 201510428586 A CN201510428586 A CN 201510428586A CN 104987437 A CN104987437 A CN 104987437A
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Abstract
The invention provides chlorinated polyethylene produced by a one-step method and a preparation method of chlorinated polyethylene. The preparation method comprises the following steps: S1, dissolving high density polyethylene in water and carrying out chlorination reaction under a condition of an emulsifier, a dispersant, an initiator and chlorine; S2, adding calcium oxide into a reaction system in the S1 in batches to generate chlorinated polyethylene resin and a calcium chloride aqueous solution; S3, centrifugalizing and drying the chlorinated polyethylene in the S2 to obtain a product chlorinated polyethylene; and S4, concentrating and drying the calcium chloride aqueous solution in the S2 to prepare a byproduct calcium chloride. Compared to a conventional process, the process flow is reduced, the occupied area and the equipment investment are reduced, and the production cost is lowered; moreover, 15 tons of water per ton of CPE can be saved and 25 tons of industrial wastewater per ton of CPE can be reduced, the water resource is saved, and the social environmental benefit is remarkable. Waste acidic water is fully utilized to prepare the byproduct. The preparation method is high in clean production level and has a relatively good economical benefit.
Description
Technical field
The invention belongs to macromolecular compound preparing technical field, particularly relate to One-step production chlorinatedpolyethylene and preparation method thereof.
Background technology
Chlorinatedpolyethylene is a kind of novel macromolecular elastomer material, has good chemical stability and a series of excellent characteristic, as: weather-proof, oil resistant, ageing-resistant, chemical-resistant resistance etc.Because containing halogen atom on the chain of chlorinatedpolyethylene, thus also there is good flame retardant properties; Again because chlorinatedpolyethylene is obtained by polyethylene chlorination, polyethylene sections containing non-chlorination in molecule, whole material presents the performance between rubber and plastics, can be widely used in the excellent properties-correcting agent of plastics and rubber, additive and specialty elastomer goods.
The preparation technology of chlorinatedpolyethylene has a variety of: one is solid phase method technology, is directly passed into by chlorine in solid polyethylene powder, in ebullated bed, directly carries out gas-solid phase reaction, because this method reaction heat not easily shifts out, be difficult to control, weight is very unstable, and seriously polluted, be progressively eliminated.Another kind is solvent method technology, is namely dissolved in carbon tetrachloride solution, passes into the homogeneous reaction after chlorine, chlorination reaction is balanced, is easy to control, and weight is also more stable, but tetracol phenixin enters air in production process, have great destruction to ozonosphere, and finished product there is tetracol phenixin to remain.
But prior art also exists technical process complexity, production unit floor space is large, and equipment investment cost is high, and blowdown acid-water can not recycle, and water resource waste is serious, the problem of contaminate environment.
Therefore, invention One-step production chlorinatedpolyethylene and preparation method thereof seems very necessary.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides One-step production chlorinatedpolyethylene and preparation method thereof, technical process complexity is there is to solve prior art, production unit floor space is large, equipment investment cost is high, blowdown acid-water can not recycle, and water resource waste is serious, the problem of contaminate environment.One-step production chlorinatedpolyethylene and preparation method thereof comprises the following steps:
, under emulsifying agent, dispersion agent, initiator and chlorine condition, there is chlorination reaction in step one: high density polyethylene(HDPE) is soluble in water;
Step 2: in batches added by calcium oxide in step one reaction system, generates chlorinated polyethylene resin and calcium chloride water;
Step 3: namely obtain product chlorinatedpolyethylene by after centrifugal for chlorinated polyethylene resin in step 2, drying;
Step 4: calcium chloride water in step 2 is obtained side product chlorinated calcium through concentrate drying.
Further, in step one, the high density polyethylene(HDPE) of 15-25 mass fraction is joined in the water of 90-100 mass fraction.
Further, in step one, described emulsifying agent is anionic species emulsifying agent and nonionic class emulsifying agent, and addition is the 1-12 ‰ of described high density polyethylene(HDPE) quality.
Further, in step one, described anionic species emulsifying agent is alkyl sulfonates emulsifying agent or alkyl alcohol sulfate class emulsifying agent; Described nonionic class emulsifying agent is polyoxyethylene base class emulsifying agent.
Further, in step one, the total amount that passes into of described chlorine is 15-25 mass parts.
Further, in step one, described dispersion agent is one or more in hydroxylated cellulose, polyolefins pyrrolidone, active silica, polyvinyl alcohol, and addition is the 6-8 ‰ of described high density polyethylene(HDPE) quality.
Further, in step one, described initiator is oil-soluble initiator, and addition is the 2.0-5.0 ‰ of described high density polyethylene(HDPE) quality; Described initiator is benzoyl peroxide, lauroyl peroxide or Diisopropyl azodicarboxylate.
Further, in step one, the temperature of reaction of described chlorination reaction is 80-135 DEG C, and the reaction times is 2-5 hour
Further, in step 2, described calcium oxide addition 4-8 mass fraction, described calcium oxide portion-wise addition speed controls at 7.0-8.0 to make the pH value of reaction system.
The obtained chlorinated polyethylene resin product of this meets national standard HG/T2704-2010 (chlorinatedpolyethylene) requirement completely, and side product chlorinated calcium product meets HG/T2327-2004 (calcium chloride) requirement completely.
Because One-step production chlorinatedpolyethylene of the present invention and preparation method thereof is widely used in macromolecular compound preparing technical field.Compared with the prior art, beneficial effect of the present invention is embodied in: simplified technical process compared with traditional technology, decreases plant area area and facility investment, reduces production cost; Simultaneously the present invention can economize on water 15 tons of/ton of CPE, and reduce discharging 25 tons of/ton of CPE trade effluents, saving water resource, social environment benefit is remarkable; Waste acid water is fully utilized, and makes byproduct, and level of clean production is high, has good economic benefit.
Accompanying drawing explanation
Fig. 1 is the production technological process of One-step production chlorinatedpolyethylene of the present invention and preparation method thereof.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described further:
In figure:
Embodiment:
As shown in Figure 1
One-step production chlorinatedpolyethylene and preparation method thereof comprises the following steps:
, under emulsifying agent, dispersion agent, initiator and chlorine condition, there is chlorination reaction in S101: high density polyethylene(HDPE) is soluble in water;
S102: in batches added by calcium oxide in S101 reaction system, generates chlorinated polyethylene resin and calcium chloride water;
S103: namely obtain product chlorinatedpolyethylene by after centrifugal for chlorinated polyethylene resin in S102, drying;
S104: calcium chloride water in S102 is obtained side product chlorinated calcium through concentrate drying.
Further, in S101, the high density polyethylene(HDPE) of 15-25 mass fraction is joined in the water of 90-100 mass fraction.
Further, in S101, described emulsifying agent is anionic species emulsifying agent and nonionic class emulsifying agent, and addition is the 1-12 ‰ of described high density polyethylene(HDPE) quality.
Further, at S101, described anionic species emulsifying agent is alkyl sulfonates emulsifying agent or alkyl alcohol sulfate class emulsifying agent; Described nonionic class emulsifying agent is polyoxyethylene base class emulsifying agent.
Further, in S101, the total amount that passes into of described chlorine is 15-25 mass parts.
Further, in S101, described dispersion agent is one or more in hydroxylated cellulose, polyolefins pyrrolidone, active silica, polyvinyl alcohol, and addition is the 6-8 ‰ of described high density polyethylene(HDPE) quality.
Further, in S101, described initiator is oil-soluble initiator, and addition is the 2.0-5.0 ‰ of described high density polyethylene(HDPE) quality; Described initiator is benzoyl peroxide, lauroyl peroxide or Diisopropyl azodicarboxylate.
Further, in S101, the temperature of reaction of described chlorination reaction is 80-135 DEG C, and the reaction times is 2-5 hour
Further, in S102, described calcium oxide addition 4-8 mass fraction, described calcium oxide portion-wise addition speed controls at 7.0-8.0 to make the pH value of reaction system.
The obtained chlorinated polyethylene resin product of this meets national standard HG/T2704-2010 (chlorinatedpolyethylene) requirement completely, and side product chlorinated calcium product meets HG/T2327-2004 (calcium chloride) requirement completely.
Because One-step production chlorinatedpolyethylene of the present invention and preparation method thereof is widely used in macromolecular compound preparing technical field.Compared with the prior art, beneficial effect of the present invention is embodied in: simplified technical process compared with traditional technology, decreases plant area area and facility investment, reduces production cost; Simultaneously the present invention can economize on water 15 tons of/ton of CPE, and reduce discharging 25 tons of/ton of CPE trade effluents, saving water resource, social environment benefit is remarkable; Waste acid water is fully utilized, and makes byproduct, and level of clean production is high, has good economic benefit.
Specific embodiment 1
Embodiment 1:
By in 4.0g Sodium dodecylbenzene sulfonate, 16.0gOP-10,20.0g polyolefine pyrrolidone (k-30), molten 2000 water of active silica 140.0g, drop into reactor, in reactor, add 2.0g benzoyl peroxide, 200.0g high density polyethylene(HDPE) successively, closed reactor, be warming up to 80 DEG C, start to pass into chlorine, when temperature is raised to 135 DEG C, add up to pass into chlorine 220.0g, stop logical chlorine, the logical 2.5 hours chlorine time, in 135 DEG C of insulation reaction 1 hour.In reaction process, add calcium oxide, the interpolation speed of calcium oxide controls to be as the criterion between 7.0-8.0 to make the pH value of reaction system, and the total amount that adds of calcium oxide is 80g in batches.During still temperature drop to 80 DEG C, purge reaction system with pressurized air, in still, material is centrifugal, solid chlorine polyethylene drying, obtains the CPE finished product of cl content 35.5%; Centrifuge mother liquor obtains content 70.1% Calcium dichloride dihydrate 120.0g through concentrated, drying.
Embodiment 2:
0.6g Sodium dodecylbenzene sulfonate, 1.4gOP-10,10.0g polyolefine pyrrolidone (k-30) are dissolved in 2000g water, drop into reactor, 10.0g benzoyl peroxide, 400.0g high density polyethylene(HDPE) closed reactor is added successively in reactor, be warming up to 80 DEG C, start to pass into chlorine, when temperature is raised to 135 DEG C, add up to pass into chlorine 210.0g, stop logical chlorine, the logical 2.5 hours chlorine time, in 135 DEG C of insulations 1 hour.In reaction process, add calcium oxide, the interpolation speed of calcium oxide controls to be as the criterion between 7.0-8.0 to make the pH value of reaction system, and the total amount that adds of calcium oxide is 160g in batches.During still temperature drop to 80 DEG C, purge reaction system with pressurized air, in still, material is centrifugal, solid chlorine polyethylene drying, obtains the CPE finished product of cl content 36.0%; Centrifuge mother liquor obtains content 90.2% calcium chloride 300g through concentrated, drying.
The result shows, present method stable processing technique is reliable, is applicable to industrialization and produces.
Utilize technical solutions according to the invention, or those skilled in the art being under the inspiration of technical solution of the present invention, designing similar technical scheme, and reach above-mentioned technique effect, is all fall into protection scope of the present invention.
Claims (9)
1. One-step production chlorinatedpolyethylene and preparation method thereof, is characterized in that, this One-step production chlorinatedpolyethylene and preparation method thereof comprises the following steps:
, under emulsifying agent, dispersion agent, initiator and chlorine condition, there is chlorination reaction in step one: high density polyethylene(HDPE) is soluble in water;
Step 2: in batches added by calcium oxide in step one reaction system, generates chlorinated polyethylene resin and calcium chloride water;
Step 3: namely obtain product chlorinatedpolyethylene by after centrifugal for chlorinated polyethylene resin in step 2, drying;
Step 4: calcium chloride water in step 2 is obtained side product chlorinated calcium through concentrate drying.
2. One-step production chlorinatedpolyethylene as claimed in claim 1 and preparation method thereof, is characterized in that, in step one, joined by the high density polyethylene(HDPE) of 15-25 mass fraction in the water of 90-100 mass fraction.
3. One-step production chlorinatedpolyethylene as claimed in claim 1 and preparation method thereof, it is characterized in that, in step one, described emulsifying agent is anionic species emulsifying agent and nonionic class emulsifying agent, and addition is the 1-12 ‰ of described high density polyethylene(HDPE) quality.
4. One-step production chlorinatedpolyethylene as claimed in claim 3 and preparation method thereof, it is characterized in that, in step one, described anionic species emulsifying agent is alkyl sulfonates emulsifying agent or alkyl alcohol sulfate class emulsifying agent; Described nonionic class emulsifying agent is polyoxyethylene base class emulsifying agent.
5. One-step production chlorinatedpolyethylene as claimed in claim 1 and preparation method thereof, it is characterized in that, in step one, the total amount that passes into of described chlorine is 15-25 mass parts.
6. One-step production chlorinatedpolyethylene as claimed in claim 1 and preparation method thereof, it is characterized in that, in step, described dispersion agent is one or more in hydroxylated cellulose, polyolefins pyrrolidone, active silica, polyvinyl alcohol, and addition is the 6-8 ‰ of described high density polyethylene(HDPE) quality.
7. One-step production chlorinatedpolyethylene as claimed in claim 1 and preparation method thereof, it is characterized in that, in step one, described initiator is oil-soluble initiator, and addition is the 2.0-5.0 ‰ of described high density polyethylene(HDPE) quality; Described initiator is benzoyl peroxide, lauroyl peroxide or Diisopropyl azodicarboxylate.
8. One-step production chlorinatedpolyethylene as claimed in claim 1 and preparation method thereof, it is characterized in that, in step one, the temperature of reaction of described chlorination reaction is 80-135 DEG C, and the reaction times is 2-5 hour.
9. One-step production chlorinatedpolyethylene as claimed in claim 1 and preparation method thereof, it is characterized in that, in step 2, described calcium oxide addition 4-8 mass fraction, described calcium oxide portion-wise addition speed controls at 7.0-8.0 to make the pH value of reaction system.
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| CN104327202A (en) * | 2014-11-12 | 2015-02-04 | 安徽省化工研究院 | One-step production method of chlorinated polyethylene |
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