CN104387514A - Alkali-based preparation method of polyacrylic acid - Google Patents
Alkali-based preparation method of polyacrylic acid Download PDFInfo
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- CN104387514A CN104387514A CN201410622589.9A CN201410622589A CN104387514A CN 104387514 A CN104387514 A CN 104387514A CN 201410622589 A CN201410622589 A CN 201410622589A CN 104387514 A CN104387514 A CN 104387514A
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Abstract
The invention discloses an alkali-based preparation method of polyacrylic acid and belongs to the technical field of organic polymers. The alkali-based preparation method of polyacrylic acid comprises the following steps: preparing a sodium polyacrylate size by using acrylic acid as a raw material, industrial water as a solvent, sodium hydroxide as an alkaline agent, and trimethylolpropane triacrylate, sodium persulfate and isoascorbate as accessories, and preparing the polyacrylic acid product having the particle diameter range of 104-1000 microns by steps of acid pickling, water washing, crushing, drying, crushing and the like. The alkali-based preparation method of the polyacrylic acid has the advantages that integrated feeding is adopted and processes such as dropwise addition are avoided, and therefore, the cost is saved, and meanwhile, the equipment utilization rate is increased, and the percent conversion of the product is increased; besides, the method is simple in process and convenient to operate.
Description
Technical field
The present invention relates to a kind of preparation method of organic polymer, particularly relate to a kind of polyacrylic alkali formula preparation method.
Background technology
Polyacrylic acid, as a kind of medicine intermediate, is usually applied to the circulation system disease that this class of heart trouble is more common.
The recycle system is by the sanguimotor neurohumour organizational composition of heart, blood vessel and adjustment, circulation system disease, also referred to as cardiovascular diseases, comprises the disease of above-mentioned all histoorgans, in internal disease, belongs to common disease, wherein common with heart trouble, the labor force of patient can be affected significantly.
Chronic pulmonary heart disease is a kind of comparatively common heart disease in China, and pathomechanism is pulmonary hypertension and high blood viscosity, and due to long term hypoxia, cause Pulmonary Vascular to shrink and cause Pulmonary vascular cell to thicken, cause microcirculation disturbance, pulmonary hypertension occurs.
Complication common is clinically acid base imbalance and electrolyte disturbance, and next has the infringement of upper gastrointestinal hemorrhage, shock, Liver and kidney function and pulmonary encephalopathy etc.
1, pulmonary encephalopathy: be one of modal severe complication of cor pulmonale is also the major reason causing patients with cor pulmonale death.
2, irregular pulse: various types of irregular pulse can appear in patients with cor pulmonale, wherein modal have paroxysmal supraventricular tachycardia and artrial premature beat.
3, acid base equilibrium and electrolyte balance disorder: the pulmonary heart disease compensatory phase, various types of acid base imbalance can appear in patient, and modal have metabolic acidosis and respiratory acidosis, and also likely several situation exists simultaneously.
It is several that electrolyte disturbance common are hyperkalemia, low blood sodium, low blood chlorine and hypokalemia.
4, digestive tract hemorrhage: the patient be in a bad way often increases due to anoxic, digestive tube extravasated blood and irritability Adrenal Glucocorticoids Secretion, and occurs digestive tube stress ulcer hemorrhage.
5, suffer a shock: Patients with Chronic Cor Pulmonale often there will be septic shock, hemorrhagic shock or cardiogenic shock.
Current research often finds heart trouble along with ionogen wadding disorderly, brings a series of complication simultaneously.
Meanwhile, control the electrolyte balance in human body, there is the effect alleviating complication, also can play good effect in cardiopathic treatment simultaneously.
Summary of the invention
The object of this invention is to provide a kind of polyacrylic alkali formula preparation method, the method production technique be simple, equipment efficiency of usage is high, speed of response is fast, less energy consumption and cost is low.This product application is in medicine intermediate, sanitary product.
A kind of polyacrylic alkali formula preparation method, it is characterized in that, it comprises the following steps:
(1) in retort, drop into vinylformic acid, then add process water, be configured to acrylic acid solution;
(2) Viscoat 295 is joined in acrylic acid solution;
(3) under agitation, joined in mixing solutions by sodium hydroxide, and control temperature of reaction, temperature range is 55 ~ 100 DEG C;
(4) Sodium persulfate is added, and continuously stirring 10 ~ 60 minutes;
(5) under agitation condition, add erythorbate, and control temperature is not higher than 70 DEG C;
(6) blend glue stuff is put into stirrer, add diluted acid agitator treating 30min, discharge diluted acid, repetitive scrubbing 2 ~ 4 times, add deionized water and stirring washing 30min in the sizing material after pickling, repetitive scrubbing 2 ~ 4 times;
(7) sizing material after washing is put on transmission arid zones, deliver to cutting machine and extruding nodulizer, be broken into tiny piece;
(8) sizing material after fragmentation is placed fluidised bed drying region dry, drying temperature is 80 ~ 200 DEG C;
(9) dried sizing material is placed in pulverizer, and then encapsulate, powder particle diameter scope is 104 ~ 1000 microns.
Further, the temperature in described step (3) is set to 90 DEG C.
Further, the temperature of reaction of described step (5) is set to 60 DEG C
Further, in described step (7), the transmission efficiency of travelling belt is 40Hz.
Further, described vinylformic acid: process water: Viscoat 295: sodium hydroxide: Sodium persulfate: the ratio of erythorbate is 692:1294:3:277:1:0.2.
Further, described erythorbate is SODIUM ISOVITAMIN C.
Further, the diluted acid in described step (6) refers to hydrochloric acid or the phosphoric acid of dilution.
Compared with prior art, the present invention has following beneficial effect:
(1) preparation method provided by the invention adopts vinylformic acid to be starting material, and water is solvent, and sodium hydroxide is alkaline agent, and material source is extensive, and observable index is lower.
(2) adopt in reaction process and integrally feed intake, without the need to adopting the techniques such as droppings, operation is relatively simple, and required equipment is eased, economic saving.
(3) method of the present invention's employing is effective fast, and substantially reduce the reaction times, plant factor substantially increases.
(4) product cut size of the inventive method is distributed as 104 ~ 1000 microns, and steady quality is reliable, and transformation efficiency is high.
Embodiment
Below in conjunction with embodiment, the present invention is described further:
Embodiment 1
A kind of polyacrylic alkali formula preparation method, it is characterized in that, it comprises the following steps:
(1) in retort, drop into 623.22kg vinylformic acid, then add 1163.76kg process water, be configured to acrylic acid solution;
(2) 2.7401kg Viscoat 295 is joined in acrylic acid solution;
(3) under agitation, joined in mixing solutions by 249.38kg sodium hydroxide, and control temperature of reaction, temperature range is 55 DEG C;
(4) 0.936kg Sodium persulfate is added, and continuously stirring 10 minutes;
(5) under agitation condition, add 0.1872kg erythorbate, and control temperature is 60 DEG C;
(6) blend glue stuff is put into stirrer, add the hydrochloric acid agitator treating 30min of dilution, discharge the hydrochloric acid of dilution, repetitive scrubbing 3 times, add deionized water and stirring washing 30min in the sizing material after pickling, repetitive scrubbing 3 times;
(7) put by the sizing material after washing on transmission arid zones, deliver to cutting machine and extruding nodulizer, be broken into tiny piece, the transmission efficiency of travelling belt is 40Hz;
(8) sizing material after fragmentation is placed fluidised bed drying region dry, drying temperature is 80 DEG C;
(9) dried sizing material is placed in pulverizer, and then encapsulate, powder particle diameter scope is 600 ~ 900 microns.
The polyacrylic particle diameter of gained is 700 microns, be 956% at the distributive law of 104-1000 micron, moisture content is 4.5%, residual monomer content is 37ppm, salt loading degree is 53g/g, and heavy metal content is less than 20ppm, and total soluble polymer content is 0.7%, lower than 1% of regulation, sodium content is less than 0.1%.
Embodiment 2
A kind of polyacrylic alkali formula preparation method, it is characterized in that, it comprises the following steps:
(1) in retort, drop into 623.22kg vinylformic acid, then add 1163.76kg process water, be configured to acrylic acid solution;
(2) 2.7401kg Viscoat 295 is joined in acrylic acid solution;
(3) under agitation, joined in mixing solutions by 249.38kg sodium hydroxide, and control temperature of reaction, temperature range is 100 DEG C;
(4) 0.936kg Sodium persulfate is added, and continuously stirring 60 minutes;
(5) under agitation condition, add 0.1872kg erythorbate, and control temperature is 70 DEG C;
(6) blend glue stuff is put into stirrer, add the phosphoric acid agitator treating 30min of dilution, discharge the phosphoric acid of dilution, repetitive scrubbing 3 times, add deionized water and stirring washing 30min in the sizing material after pickling, repetitive scrubbing 3 times;
(7) put by the sizing material after washing on transmission arid zones, deliver to cutting machine and extruding nodulizer, be broken into tiny piece, the transmission efficiency of travelling belt is 40Hz;
(8) sizing material after fragmentation is placed fluidised bed drying region dry, drying temperature is 200 DEG C;
(9) dried sizing material is placed in pulverizer, and then encapsulate, powder particle diameter scope is 300 ~ 800 microns.
The polyacrylic particle diameter of gained is 500 microns, be 94% at the distributive law of 104-1000 micron, moisture content is 4.7%, residual monomer content is 44ppm, salt loading degree is 43g/g, and heavy metal content is less than 20ppm, and total soluble polymer content is 0.5%, lower than 1% of regulation, sodium content is less than 0.1%.
Embodiment 3
A kind of polyacrylic alkali formula preparation method, it is characterized in that, it comprises the following steps:
(1) in retort, drop into 1246kg vinylformic acid, then add 2328kg process water, be configured to acrylic acid solution;
(2) 5.48kg Viscoat 295 is joined in acrylic acid solution;
(3) under agitation, joined in mixing solutions by 499kg sodium hydroxide, and control temperature of reaction, temperature range is 90 DEG C;
(4) 1.87kg Sodium persulfate is added, and continuously stirring 40min;
(5) under agitation condition, add 0.37kg erythorbate, and control temperature is 50 DEG C;
(6) blend glue stuff is put into stirrer, add the phosphoric acid agitator treating 30min of dilution, discharge the phosphoric acid of dilution, repetitive scrubbing 4 times, add deionized water and stirring washing 30min in the sizing material after pickling, repetitive scrubbing 4 times;
(7) put by the sizing material after washing on transmission arid zones, deliver to cutting machine and extruding nodulizer, be broken into tiny piece, the transmission efficiency of travelling belt is 40Hz;
(8) sizing material after fragmentation is placed fluidised bed drying region dry, drying temperature is 130 DEG C;
(9) dried sizing material is placed in pulverizer, and then encapsulate, powder particle diameter scope is 300 ~ 1000 microns.
The polyacrylic particle diameter of gained is 700 microns, be 93% at the distributive law of 104-1000 micron, moisture content is 4.2%, residual monomer content is 33ppm, salt loading degree is 45g/g, and heavy metal content is less than 20ppm, and total soluble polymer content is 0.8%, lower than 1% of regulation, sodium content is less than 0.1%.
The foregoing is only some embodiments of the present invention, do not limit the present invention, the technical scheme that the mode that all employings are equal to replacement or equivalent transformation obtains, all drop in protection scope of the present invention.
Claims (7)
1. a polyacrylic alkali formula preparation method, it is characterized in that, it comprises the following steps:
(1) in retort, drop into vinylformic acid, then add process water, be configured to acrylic acid solution;
(2) Viscoat 295 is joined in acrylic acid solution;
(3) under agitation, joined in mixing solutions by sodium hydroxide, and control temperature of reaction, temperature range is 55 ~ 100 DEG C;
(4) Sodium persulfate is added, and continuously stirring 10 ~ 60 minutes;
(5) under agitation condition, add erythorbate, and control temperature is not higher than 70 DEG C;
(6) blend glue stuff is put into stirrer, add diluted acid agitator treating 30min, discharge diluted acid, repetitive scrubbing 2 ~ 4 times, add deionized water and stirring washing 30min in the sizing material after pickling, repetitive scrubbing 2 ~ 4 times;
(7) sizing material after washing is put on transmission arid zones, deliver to cutting machine and extruding nodulizer, be broken into tiny piece;
(8) sizing material after fragmentation is placed fluidised bed drying region dry, drying temperature is 80 ~ 200 DEG C;
(9) dried sizing material is placed in pulverizer, and then encapsulate, powder particle diameter scope is 104 ~ 1000 microns.
2. one according to claim 1 polyacrylic alkali formula preparation method, is characterized in that: the temperature in described step (3) is set to 90 DEG C.
3. one according to claim 1 polyacrylic alkali formula preparation method, is characterized in that: the temperature of reaction of described step (5) is set to 60 DEG C.
4. one according to claim 1 polyacrylic alkali formula preparation method, is characterized in that: in described step (7), the transmission efficiency of travelling belt is 40Hz.
5. one according to claim 1 polyacrylic alkali formula preparation method, is characterized in that: described vinylformic acid: process water: Viscoat 295: sodium hydroxide: Sodium persulfate: the ratio of saccharosonic acid is 692:1294:3:277:1:0.2.
6. one according to claim 1 polyacrylic alkali formula preparation method, is characterized in that: described erythorbate is SODIUM ISOVITAMIN C.
7. one according to claim 1 polyacrylic alkali formula preparation method, is characterized in that: the diluted acid in described step (6) is hydrochloric acid or the phosphoric acid of dilution.
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| CN201410622589.9A CN104387514A (en) | 2014-11-08 | 2014-11-08 | Alkali-based preparation method of polyacrylic acid |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872890A (en) * | 2006-06-30 | 2006-12-06 | 上海华谊丙烯酸有限公司 | Method for preparing high absorptive resin in acrylic acid type |
| CN101094696A (en) * | 2004-12-30 | 2007-12-26 | 巴斯福股份公司 | Superabsorbent polymer particles having a reduced amount of fine-sized particles, and methods of manufacturing the same |
| CN101100493A (en) * | 2007-06-29 | 2008-01-09 | 上海华谊丙烯酸有限公司 | Method for fast preparing high water absorption resin |
| WO2008037672A1 (en) * | 2006-09-25 | 2008-04-03 | Basf Se | Method for the classification of water absorbent polymer particles |
| CN104114591A (en) * | 2012-02-15 | 2014-10-22 | 巴斯夫欧洲公司 | Water-absorbing polymer particles having a high swelling rate and high permeability |
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- 2014-11-08 CN CN201410622589.9A patent/CN104387514A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101094696A (en) * | 2004-12-30 | 2007-12-26 | 巴斯福股份公司 | Superabsorbent polymer particles having a reduced amount of fine-sized particles, and methods of manufacturing the same |
| CN1872890A (en) * | 2006-06-30 | 2006-12-06 | 上海华谊丙烯酸有限公司 | Method for preparing high absorptive resin in acrylic acid type |
| WO2008037672A1 (en) * | 2006-09-25 | 2008-04-03 | Basf Se | Method for the classification of water absorbent polymer particles |
| CN101100493A (en) * | 2007-06-29 | 2008-01-09 | 上海华谊丙烯酸有限公司 | Method for fast preparing high water absorption resin |
| CN104114591A (en) * | 2012-02-15 | 2014-10-22 | 巴斯夫欧洲公司 | Water-absorbing polymer particles having a high swelling rate and high permeability |
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Application publication date: 20150304 |