CN1099762A - Method for preparing hydrolytic maleic anhydride - Google Patents
Method for preparing hydrolytic maleic anhydride Download PDFInfo
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- CN1099762A CN1099762A CN 93112137 CN93112137A CN1099762A CN 1099762 A CN1099762 A CN 1099762A CN 93112137 CN93112137 CN 93112137 CN 93112137 A CN93112137 A CN 93112137A CN 1099762 A CN1099762 A CN 1099762A
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- hpma
- maleic anhydride
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Abstract
This invention discloses a preparation method for hydrolytic polymaelic anhydride (HPMA) of water treating agent. The said method is as follows: maleic anhydride is melted by heating, controlling a certain temp., introducing H2O2 initiator for polymerization so that HPMA is made up and its quality indices conforms to the requirement of GB10535-89. This method has simple technology, no pollution, high productivity, low investment, and easy realization of industrialization.
Description
The invention relates to the preparation method of a kind of water conditioner hydrolytic polymaleic anhydride (HPMA).
HPMA be 1971 at first by the success of Switzerland CIBA-GEIGY company suitability for industrialized production, and priority is used for treatment of cooling water and sea water desaltination is handled, this product has good prevention calcium carbonate scale, disperses the performance of calcium phosphate scale, and is high temperature resistant in addition, nontoxic simultaneously, be used the good characteristics such as corrosion inhibition that produce with zinc salt.China also began to produce HPMA in 1979, and was mainly used in boiler water processing, was used for the processing of water coolant, oil-field water on a small quantity, but because the production cost of general production method is too high, had limited the large-scale promotion application of HPMA.
At present, it is initiator that benzoyl peroxide is generally adopted in the preparation of HPMA, carries out the solution precipitation polymerization in organic solvent such as toluene, dimethylbenzene, treatedly then again polymaleic anhydride is hydrolyzed to HPMA.The used initiator of this method costs an arm and a leg, and consumption is big; Employed organic solvent is poisonous, and consumption is also big, and used solvent also must distill and reclaim usefulness again, complex process, and facility investment is big, causes production cost higher.Therefore, the investigator develops new preparation method in searching both at home and abroad, to reduce production costs.Japanese Patent JP86 178 097 once proposed the aqueous solution polymerization method of toxilic acid, but initiator amount is big, and the product that obtains is single sodium salt of polymaleic acid.
It is simple to the objective of the invention is to seek a kind of technology, does not use deleterious organic solvent, and facility investment is little, the HPMA preparation method that cost is low.
The objective of the invention is to realize by following method.
This law is controlled certain temperature at first with the maleic anhydride heat fused, adds initator H then under constantly stirring
2O
2, after initator adds, the insulation reaction certain hour, thin up, cooling namely gets the HPMA product.
When preparing HPMA with said method, need the control reaction temperature, H
2O
2Dosage, H
2O
2The adding mode, insulation reaction time, amount of water etc.The present invention controls following technical qualification:
Temperature of reaction is controlled between 90-140 ℃.
Initator H
2O
2The adding mode is for dripping, and time for adding was advisable with about 5 hours.
Initator H
2O
2(30.0% the aqueous solution) consumption accounts for the 50-100% of maleic anhydride weight.
Insulation reaction was kept about 105 ℃ about 2 hours.
The density of HPMA product can be regulated by thin up, generally is controlled at 1.21-1.23g/cm
3(20 ℃) are advisable, and this moment, the product solid content was about 50%.
With the HPMA of method for preparing, product quality indicator reaches the standard-required of GB10535-89.
Advantages such as the present invention compares with existing HPMA preparation method, and it is simple to have production technique, pollution-free, and initiator is cheap and easy to get, and the production time is short, and whole process of preparation is finished in a still, and production cost is low.
Embodiment 1: add the 490g maleic anhydride in the 1L four-hole bottle, heating makes its fusing, is warmed up to 140 ℃, drips then the H of 490g30%
2O
2, dripped off in 5 hours, temperature is down to 103 ℃, insulation is 2 hours under this temperature, adds 170g water, lower the temperature the 1000gHPMA product.
Embodiment 2: add the 490g maleic anhydride in the 1L four-hole bottle, heating makes its fusing, is warmed up to 125 ℃, begins then to drip the H of 400g30%
2O
2, dripped off in 5 hours, temperature is down to 104 ℃, insulation is 2 hours under this temperature, adds 260g water, lower the temperature the 1000gHPMA product.
Embodiment 3: add the 490g maleic anhydride in the 1L four-hole bottle, heating makes its fusing, is warming up to 90 ℃, drips the H of 250g30%
2O
2, the control temperature surpasses 130 ℃ in whole dropping process, drips off in 5 hours, temperature is down to 106 ℃ at last, insulation is 2 hours under this temperature, adds 400g water, lower the temperature the 1000gHPMA product.
The leading indicator of above-mentioned three embodiment gained HPMA is as follows:
| Index name | Index |
| Solids content, % mean molecule quantity (number average), 〉=bromine number, mg/g, ≤ pH value (1% aqueous solution) density, g/cm 3(20 ℃) | 50.0 ± 2.0 300 120.0 2.0-3.0 1.21-1.23 |
Claims (5)
1, a kind of method for preparing HPMA (HPMA) is characterized in that at first the maleic anhydride heat fused is controlled certain temperature, is adding H then under constantly stirring
2O
2Initiated polymerization, afterwards, the insulation reaction certain hour, cooling namely gets the HPMA product.
2, the method for claim 1, temperature of reaction are controlled at 90-140 ℃.
3, the method for claim 1, initator H
2O
2The adding mode for dripping, time for adding is about 5 hours.
4, such as claim 1,3 described methods, initator H
2O
2Consumption be that the 50-100%(of maleic anhydride weight is with 30% H
2O
2Meter).
5, the method for claim 1, insulation reaction were kept about 105 ℃ about 2 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93112137 CN1099762A (en) | 1993-08-30 | 1993-08-30 | Method for preparing hydrolytic maleic anhydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93112137 CN1099762A (en) | 1993-08-30 | 1993-08-30 | Method for preparing hydrolytic maleic anhydride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1099762A true CN1099762A (en) | 1995-03-08 |
Family
ID=4989870
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93112137 Pending CN1099762A (en) | 1993-08-30 | 1993-08-30 | Method for preparing hydrolytic maleic anhydride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1099762A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638307A (en) * | 2009-09-08 | 2010-02-03 | 邢献军 | Novel plastering mortar |
| CN101575392B (en) * | 2009-06-24 | 2011-09-14 | 安徽省蓝天化工有限公司 | Preparation method of polymaleic acid |
| CN102766235A (en) * | 2011-05-06 | 2012-11-07 | 江苏大明科技有限公司 | Synthesis technology of hydrolytic polymaleic anhydride |
-
1993
- 1993-08-30 CN CN 93112137 patent/CN1099762A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575392B (en) * | 2009-06-24 | 2011-09-14 | 安徽省蓝天化工有限公司 | Preparation method of polymaleic acid |
| CN101638307A (en) * | 2009-09-08 | 2010-02-03 | 邢献军 | Novel plastering mortar |
| CN102766235A (en) * | 2011-05-06 | 2012-11-07 | 江苏大明科技有限公司 | Synthesis technology of hydrolytic polymaleic anhydride |
| CN102766235B (en) * | 2011-05-06 | 2015-01-28 | 江苏大明科技有限公司 | Synthesis technology of hydrolytic polymaleic anhydride |
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| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |