CN101747472A - Method for preparing high molecular weight instant cationic flocculant - Google Patents
Method for preparing high molecular weight instant cationic flocculant Download PDFInfo
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- CN101747472A CN101747472A CN200810243756A CN200810243756A CN101747472A CN 101747472 A CN101747472 A CN 101747472A CN 200810243756 A CN200810243756 A CN 200810243756A CN 200810243756 A CN200810243756 A CN 200810243756A CN 101747472 A CN101747472 A CN 101747472A
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Abstract
The invention provides a method for preparing high molecular weight instant cationic flocculant. The method comprises the following steps: adding acrylamide, acryloyloxyethyl trimethyl ammonium chloride and methacrylatoethyl trimethyl ammonium chloride to a proportioning kettle and mixing the three well; adding silica; adding organic acid and deionized water; ensuring that the total concentration of the sum of acrylamide, acryloyloxyethyl trimethyl ammonium chloride and methacrylatoethyl trimethyl ammonium chloride to reach 28 to 40 percent; cooling to 0 DEG C; regulating pH to between 1 and 5; complete proportioning; transferring proportioned materials into a reaction kettle; adding chelating agent, chain transfer agent and oxidant; feeding nitrogen and stirring; adding oxidant and reducing agent, continuing feeding nitrogen, stopping feeding nitrogen and sealing; performing adiabatic polymerization for 1.5 to 2.5 hours; opening the reaction kettle; extruding rubber blocks by use of compressed air; and obtaining finished products through granulation, drying, grinding and screening. The products prepared by the method have the advantages of high molecular weight, good water solubility and high dissolution speed.
Description
Technical field
The present invention relates to a kind of preparation method of high molecular weight instant cationic flocculant, belong to the synthetic field of water-soluble polymer.
Background technology
Along with the requirement of social sustainable development with set up the needs of recycling economy, country constantly strengthens particularly waste water control dynamics of environmental improvement, mostly traditional flocculation agent that is used for waste water control is the flocculation agent that some are inorganic, as polymerize aluminum chloride, bodied ferric sulfate etc., these handle medicament, and not only consumption is big, the mud loose volume is big, be difficult to handle, and flocculating effect is unsatisfactory.The organic polymer coargulator that uses has had bigger improvement than inorganic flocculating agent treatment effect in water treatment at present, particularly cationic polyacrylamide class flocculation agent range of application more and more widely, but, existing cationic flocculant majority is to adopt acrylamide and a kind of cationic monomer copolymerization synthetic, molecular weight is little, cationic degree is low, dissolution rate slow (being difficult to molten entirely in 2 hours), use range is narrow, and the floc sedimentation that forms is loose, and is broken easily, and the water content of mud is big, be difficult for pressing mud, be difficult to satisfy highly difficult wastewater treatment requirement.
Summary of the invention
Low in order to solve existing cationic polyacrylamide class flocculating agent molecule amount, use range is narrow, dissolution rate is slow, be difficult to satisfy the problem of highly difficult wastewater treatment requirement, the object of the present invention is to provide a kind of preparation method of high molecular weight instant type cationic flocculant,, good water solubility adjustable as required by product relative molecular weight height, cationic charge density height, the cationic degree of the preparation of this method, dissolution rate are fast.
The technical scheme that realizes the object of the invention is as follows:
A kind of preparation method of high molecular weight instant cationic flocculant, may further comprise the steps: by weight with 1～9.8 part of acrylamide, 0.1～8.9 part of acrylyl oxy-ethyl-trimethyl salmiac, 0.1～8.9 part of methylacryoyloxyethyl trimethyl ammonium chloride, join thorough mixing in the batching still, the silicon-dioxide that adds three's total amount 0.5～1% simultaneously, the organic acid that adds three's total amount 0.1～5% again, add deionized water, make acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, the total concn of methylacryoyloxyethyl trimethyl ammonium chloride sum reaches 28%～40%, be cooled to 0 ℃, regulate pH value to 1～5 with acid, finish batching; The material for preparing is transferred in the reactor, a flat iron plate for making cakes mixture, chain-transfer agent, oxygenant are added in the reactor, logical nitrogen stirred after 10～30 minutes, added Oxidizing and Reducing Agents again and continued logical nitrogen and stop nitrogen after 10～30 minutes and seal adiabatic polymerisation reaction 1.5～2.5 hours; Open the reactor bottom valve after 2～4 hours, extrude blob of viscose, obtain finished product through granulation, drying, pulverizing, screening with pressurized air.
The a flat iron plate for making cakes mixture is a disodium ethylene diamine tetraacetate, and chain-transfer agent is a sodium hypophosphite; Oxygenant is Sodium Persulfate, azo NSC 18620 hydrochloride, Diisopropyl azodicarboxylate, reductive agent is sodium bisulfite, cuprous chloride, and they are respectively with the mass ratio of total dosage in reactor: disodium ethylene diamine tetraacetate 50～200ppm, sodium hypophosphite 10～50ppm, Sodium Persulfate 1～10ppm, azo NSC 18620 hydrochloride 10～100ppm, Diisopropyl azodicarboxylate 300～800ppm, sodium bisulfite 20～30ppm, cuprous chloride 5～20ppm.
Regulating the used weak acid of pH value is phosphoric acid, and the preferred values of pH value is 4～5.
The organic acid that adds is citric acid or maleic acid or FUMARIC ACID TECH GRADE.
The present invention adopts the composite initiation system segmentation of Oxidizing and Reducing Agents to cause, reduced the polymerization kick off temperature, it is more even that system forms free radical, polyreaction and temperature rise are all compared evenly like this, polymeric reaction temperature-time curve makes progress gently, this reaction process helps chainpropagation, can obtain the bigger product of molecular weight ratio, simultaneously because reaction is even, molecular chain is straight chain type substantially, and its dissolution rate is fast, and dissolution time is short, and be not easy to occur water-insoluble, and it is crosslinked to guarantee that branching does not appear in product in the high-temperature zone.
Polymerization-filling concentration is 28～40%, this is to produce the unapproachable concentration of polyacrylamide (general polyacrylamide production concentration is below 23%), it mainly is to solve two technical barriers that the present invention adopts so high polymerization concentration, the one, and (polymeric kettle can reach 13m in big still polymerization
3) a sticking still difficult problem; The 2nd, make not granulating, and the difficult problem of sticking drying bed.
Adopt 2 kinds of cationic monomer-acrylyl oxy-ethyl-trimethyl salmiacs and methylacryoyloxyethyl trimethyl ammonium chloride to participate in polymerization, overcome single cationic monomer and participated in defectives such as polymeric product use range is narrow, floc sedimentation is loose in some water, race mud.
The adding of auxiliary agent silicon-dioxide helps accelerating the dissolution rate of product, is beneficial to granulation, sticking bed when helping alleviating drying and high temperature degradation when high and dry.
The product that adopts method provided by the invention to obtain, molecular weight is between 500～2,000 ten thousand, and product is soluble in water.
Embodiment
Further specify the present invention below in conjunction with several embodiment.
Embodiment 1:
A, in the batching still, squeeze into 1343 kilograms of acrylamides (folding 100%) with pump, 270 kilograms of acrylyl oxy-ethyl-trimethyl salmiacs, 30 kilograms of methylacryoyloxyethyl trimethyl ammonium chlorides, 5 kilograms of silica 1s, 10 kilograms of citric acids add water to cumulative volume 5m
3, unlatching mixes, and is cooled to 0 ℃ with chilled brine simultaneously, with phosphoric acid regulating ph value to 2.9, finishes batching;
B, the feed liquid for preparing is pumped into polymeric kettle, add a flat iron plate for making cakes mixture-disodium ethylene diamine tetraacetate 835 grams (167ppm), chain-transfer agent-sodium hypophosphite 100 grams (20ppm), oxygenant-azo NSC 18620 hydrochloride 400 grams (80ppm), Diisopropyl azodicarboxylate 2500 grams (500ppm), logical nitrogen (0.4～0.6MPa) 20 minute, then, add oxygenant-persulfuric acid and receive 30 grams (6ppm), add reductive agent-sodium bisulfite 110 grams (22ppm) after 5 minutes, add reductive agent-cuprous chloride 40 grams (8ppm) after 1 minute, continue logical nitrogen (0.4～0.6MPa), stopping nitrogen after 15 minutes seals, adiabatic polymerisation reaction 1.5 hours, temperature rises to 89.6 ℃;
C, placement extruded the blob of viscose that reaction generates with pressurized air (0.3MPa) after 3 hours;
D, with blob of viscose granulation, drying, pulverizing, screening, obtain 20～80 orders, molecular weight 1,560 ten thousand (measuring) by GB, cationic degree (colloid titration method) is 12.8% white powder cationic flocculant product, its dissolving does not have insolubles after 20 minutes substantially, filters no insolubles with the G2 funnel after 30 minutes.
Embodiment 2:
A, in the batching still, squeeze into 950 kilograms of acrylamides (folding 100%) with pump, 50 kilograms of acrylyl oxy-ethyl-trimethyl salmiacs, 400 kilograms of methylacryoyloxyethyl trimethyl ammonium chlorides, 3 kilograms of silica 1s, 10 kilograms of FUMARIC ACID TECH GRADE add water to cumulative volume 5m
3, unlatching mixes, and is cooled to 0 ℃ with chilled brine simultaneously, regulates PH to 3.7 with phosphoric acid, finishes batching;
B, the feed liquid for preparing is pumped into polymeric kettle, add a flat iron plate for making cakes mixture-disodium ethylene diamine tetraacetate 750 grams (150ppm), chain-transfer agent-sodium hypophosphite 115 grams (23ppm), oxygenant-azo NSC 18620 hydrochloride 358 grams (71.6ppm), Diisopropyl azodicarboxylate 2800 grams (560ppm), logical nitrogen (0.4～0.6MPa) 20 minute, then, add oxygenant-persulfuric acid and receive 45 grams (9ppm), add reductive agent-sodium bisulfite 125 grams (25ppm) after 5 minutes, add reductive agent-cuprous chloride 60 grams (12ppm) after 1 minute, continue logical nitrogen (0.4～0.6MPa), stopping nitrogen after 15 minutes seals, adiabatic polymerisation reaction 2 hours, temperature rises to 87 ℃;
C, placement extruded the blob of viscose that reaction generates with pressurized air (0.3MPa) after 2 hours;
D, with blob of viscose granulation, drying, pulverizing, screening, obtain 20～80 orders, molecular weight 1,245 ten thousand (measuring) by GB, cationic degree (colloid titration method) is 25.4% white powder cationic flocculant product.
Embodiment 3:
A, in batching still jar, squeeze into 600 kilograms of acrylamides (folding 100%) with pump, 1000 kilograms of acrylyl oxy-ethyl-trimethyl salmiacs, 200 kilograms of methylacryoyloxyethyl trimethyl ammonium chlorides, 0 kilogram of silica 1,10 kilograms of maleic acids add water to cumulative volume 5m
3, unlatching mixes, and is cooled to 0 ℃ with chilled brine simultaneously, with phosphoric acid regulating ph value to 4.5, finishes batching;
B, the feed liquid for preparing is pumped into polymeric kettle, add a flat iron plate for making cakes mixture-disodium ethylene diamine tetraacetate 425 grams (85ppm), chain-transfer agent-sodium hypophosphite 140 grams (28ppm), oxygenant-azo NSC 18620 hydrochloride 450 grams (90ppm), Diisopropyl azodicarboxylate 3000 grams (600ppm), logical nitrogen (0.4～0.6MPa) 20 minute, then, add oxygenant-persulfuric acid and receive 50 grams (10ppm), add reductive agent-sodium bisulfite 130 grams (26ppm) after 5 minutes, add reductive agent-cuprous chloride 75 grams (15ppm) after 1 minute, continue logical nitrogen (0.4～0.6MPa), stopping nitrogen after 15 minutes seals, adiabatic polymerisation reaction 2 hours, temperature rises to 85.6 ℃;
C, placement extruded the blob of viscose that reaction generates with pressurized air (0.3MPa) after 2.5 hours;
D, with blob of viscose granulation, drying, pulverizing, screening, obtain 20～80 orders, molecular weight 8,450,000 (measuring) by GB, cationic degree (colloid titration method) is 58.7% white powder cationic flocculant product.
Claims (4)
1. the preparation method of a high molecular weight instant cationic flocculant, it is characterized in that may further comprise the steps: by weight with 1～9.8 part of acrylamide, 0.1～8.9 part of acrylyl oxy-ethyl-trimethyl salmiac, 0.1～8.9 part of methylacryoyloxyethyl trimethyl ammonium chloride, join thorough mixing in the batching still, the silicon-dioxide that adds three's total amount 0.5～1% simultaneously, the organic acid that adds three's total amount 0.1～5% again, add deionized water, make acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, the total concn of methylacryoyloxyethyl trimethyl ammonium chloride sum reaches 28%～40%, be cooled to 0 ℃, regulate pH value to 1～5 with acid, finish batching; The material for preparing is transferred in the reactor, a flat iron plate for making cakes mixture, chain-transfer agent, oxygenant are added in the reactor, logical nitrogen stirred after 10～30 minutes, added Oxidizing and Reducing Agents again and continued logical nitrogen and stop nitrogen after 10～30 minutes and seal adiabatic polymerisation reaction 1.5～2.5 hours; Open the reactor bottom valve after 2～4 hours, extrude blob of viscose, obtain finished product through granulation, drying, pulverizing, screening with pressurized air.
2. the preparation method of high molecular weight instant cationic flocculant according to claim 1, it is characterized in that: a flat iron plate for making cakes mixture is a disodium ethylene diamine tetraacetate, chain-transfer agent is a sodium hypophosphite; Oxygenant is Sodium Persulfate, azo NSC 18620 hydrochloride, Diisopropyl azodicarboxylate, reductive agent is sodium bisulfite, cuprous chloride, and they are respectively with the mass ratio of total dosage in reactor: disodium ethylene diamine tetraacetate 50～200ppm, sodium hypophosphite 10～50ppm, Sodium Persulfate 1～10ppm, azo NSC 18620 hydrochloride 10～100ppm, Diisopropyl azodicarboxylate 300～800ppm, sodium bisulfite 20～30ppm, cuprous chloride 5～20ppm.
3. the preparation method of high molecular weight instant cationic flocculant according to claim 1 is characterized in that: regulating the used acid of pH value is phosphoric acid, and the preferred values of pH value is 4～5.
4. the preparation method of high molecular weight instant cationic flocculant according to claim 1, it is characterized in that: the organic acid of adding is citric acid or maleic acid or FUMARIC ACID TECH GRADE.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242489A (en) * | 2013-05-20 | 2013-08-14 | 安徽天润化学工业股份有限公司 | Preparation method of settling separation agent for red mud in aluminium ores |
| CN103772606A (en) * | 2014-01-24 | 2014-05-07 | 安徽天润化学工业股份有限公司 | Preparation method of polyacrylamide for retention and drainage of papermaking |
| CN104245763A (en) * | 2012-04-13 | 2014-12-24 | 巴斯夫欧洲公司 | New cationic polymers |
| CN108128872A (en) * | 2017-12-29 | 2018-06-08 | 山东诺尔生物科技有限公司 | A kind of ultra-fine tailing pretreating agent and its preparation method and application |
| CN112480310A (en) * | 2020-12-08 | 2021-03-12 | 爱森（中国）絮凝剂有限公司 | Cross-linked cationic polyacrylamide sludge dehydrating agent and preparation method thereof |
| CN114349901A (en) * | 2021-12-15 | 2022-04-15 | 常州市振邦化工制造有限公司 | Preparation method of flocculant |
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2008
- 2008-12-15 CN CN200810243756A patent/CN101747472A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104245763A (en) * | 2012-04-13 | 2014-12-24 | 巴斯夫欧洲公司 | New cationic polymers |
| CN103242489A (en) * | 2013-05-20 | 2013-08-14 | 安徽天润化学工业股份有限公司 | Preparation method of settling separation agent for red mud in aluminium ores |
| CN103772606A (en) * | 2014-01-24 | 2014-05-07 | 安徽天润化学工业股份有限公司 | Preparation method of polyacrylamide for retention and drainage of papermaking |
| CN108128872A (en) * | 2017-12-29 | 2018-06-08 | 山东诺尔生物科技有限公司 | A kind of ultra-fine tailing pretreating agent and its preparation method and application |
| CN108128872B (en) * | 2017-12-29 | 2021-01-12 | 山东诺尔生物科技有限公司 | Pretreating agent for superfine tailing, and preparation method and application thereof |
| CN112480310A (en) * | 2020-12-08 | 2021-03-12 | 爱森（中国）絮凝剂有限公司 | Cross-linked cationic polyacrylamide sludge dehydrating agent and preparation method thereof |
| CN112480310B (en) * | 2020-12-08 | 2022-10-28 | 爱森（中国）絮凝剂有限公司 | Cross-linked cationic polyacrylamide sludge dehydrating agent and preparation method thereof |
| CN114349901A (en) * | 2021-12-15 | 2022-04-15 | 常州市振邦化工制造有限公司 | Preparation method of flocculant |
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Open date: 20100623 |