CN102259842A - Preparation method of hydrophobic trisodium phosphate dodecahydrate - Google Patents
Preparation method of hydrophobic trisodium phosphate dodecahydrate Download PDFInfo
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- CN102259842A CN102259842A CN2011101730597A CN201110173059A CN102259842A CN 102259842 A CN102259842 A CN 102259842A CN 2011101730597 A CN2011101730597 A CN 2011101730597A CN 201110173059 A CN201110173059 A CN 201110173059A CN 102259842 A CN102259842 A CN 102259842A
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Abstract
The invention relates to a preparation method of hydrophobic trisodium phosphate dodecahydrate. The preparation method is characterized by comprising the following steps of: adding appropriate phosphoric acid solution into a neutralization kettle, then regulating mass percentage concentration to be 35-40% with running water; then neutralizing with appropriate sodium hydroxide solution until pH value of neutralized solution is 11.5-12.5, and maintaining reaction temperature to be 80-85 DEG C; filtering the neutralized solution after reaction is completed, inputting filtrate into a crystallization kettle, adding sodium phosphate into the filtrate according to the standard that 2-3kg of sodium phosphate is added into the pre cubic meter of the filtrate when temperature of the filtrate reaches 65 DEG C, cooling, completing crystallization, discharging after the temperature in the crystallization kettle is reduced to 30 DEG C, carrying out centrifugal separation, and drying to obtain the product. In the preparation method of hydrophobic trisodium phosphate dodecahydrate provided by the invention, a preparation process is optimized, and crystallization promoter is added, thus grain size and size distribution of the product can be controlled, better appearance and surface hydrophobicity are obtained, and caking of the product is effectively inhibited.
Description
Technical field
The present invention relates to a kind of preparation method of hydrophobicity ten phosphate dihydrate trisodiums, belong to field of fine chemical.
Background technology
12 hypophosphite monohydrate trisodium Na
3PO
412H
2O: molecular weight 380.14, colourless, octahedron, isometric system, relative density 1.62, fusing point 73.40, easy-weathering in dry air is dissolved in the crystal water own, is insoluble in CS 2, the ethanol, and the aqueous solution is alkalescence, and slight corrodibility is arranged.In industries such as chemical industry, weaving, printing and dyeing, papermaking, generating, be used as water-softening chemicals and washing composition.Can make the scale inhibitor of boiler again, the metal-derusting agent, the juice purification agent, the peptizer of rubber latex and fabric mercerising toughener etc. can be used as foodstuff additive in food service industry, be broad-spectrum Chemicals.
Ten phosphate dihydrate trisodiums of the prior art are to be that 70% phosphoric acid and concentration are that 32% caustic soda reacts by a certain percentage and generates Sodium phosphate dibasic liquid by concentration, through concentrate, formation solid crystal particle after the crystallization.Its defective is: agglomeration problems is arranged when producing ten phosphate dihydrate trisodiums with aforesaid method, the ten phosphate dihydrate trisodiums that new production is come out are deposited about 10～15 days and will be formed a monoblock, need the people for breaking processing into pieces, break into pieces and deposit after one day caking again after the processing, with the wind conveying products time, latch up phenomenon in the airduct road, also occurs, influence the normal use of equipment.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, and a kind of new, preparation method that technology more rationally, effectively prevents the hydrophobicity ten phosphate dihydrate trisodiums of finished product caking is provided.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is a kind of preparation method of hydrophobicity ten phosphate dihydrate trisodiums, is characterized in, the steps include: with an amount of mass percent concentration to be that being transferred to mass percent concentration with tap water is 35 ~ 40% during 75 ~ 85% phosphoric acid solution is put into and in the still; Be the neutralization of 30% sodium hydroxide solution with an amount of mass percent concentration then,, keep 80 ~ 85 ℃ of temperature of reaction up to neutralizer pH=11.5 ~ 12.5; The neutralizer that reaction is finished filters, and filtrate is input in the crystallization kettle, when the filtrate temperature reaches 65 ℃, by 2 ~ 3kg/m
3In filtrate, add sodium phosphate, cooling, crystallization is finished, discharging after the crystallization temperature in the kettle drops to 30 ℃, centrifugation, dry, product.
Compared with prior art, adopt the inventive method production hydrophobicity ten phosphate dihydrate trisodiums,, make the particle diameter and the controllable size distribution of product by the method for optimal preparation technology and interpolation crystallization in motion agent sodium phosphate, obtain reasonable pattern and surface hydrophobicity, thereby suppress the caking of product effectively.
Embodiment
Below further describe concrete technical scheme of the present invention,, and do not constitute restriction its right so that those skilled in the art understands the present invention further.
Embodiment 1, and a kind of preparation method of hydrophobicity ten phosphate dihydrate trisodiums the steps include: with an amount of mass percent concentration to be that being transferred to mass percent concentration with tap water is 35% during 75% phosphoric acid solution is put into and in the still; Be the neutralization of 30% sodium hydroxide solution with an amount of mass percent concentration then,, keep 80 ℃ of temperature of reaction up to neutralizer pH=11.5; The neutralizer that reaction is finished filters, and filtrate is input in the crystallization kettle, when the filtrate temperature reaches 65 ℃, presses 2kg/m
3In filtrate, add sodium phosphate, cooling, crystallization is finished, discharging after the crystallization temperature in the kettle drops to 30 ℃, centrifugation, dry, product.
Embodiment 2, and a kind of preparation method of hydrophobicity ten phosphate dihydrate trisodiums the steps include: with an amount of mass percent concentration to be that being transferred to mass percent concentration with tap water is 40% during 85% phosphoric acid solution is put into and in the still; Be the neutralization of 30% sodium hydroxide solution with an amount of mass percent concentration then,, keep 85 ℃ of temperature of reaction up to neutralizer pH=12.5; The neutralizer that reaction is finished filters, and filtrate is input in the crystallization kettle, when the filtrate temperature reaches 65 ℃, presses 3kg/m
3In filtrate, add sodium phosphate, cooling, crystallization is finished, discharging after the crystallization temperature in the kettle drops to 30 ℃, centrifugation, dry, product.
Embodiment 3.A kind of preparation method of hydrophobicity ten phosphate dihydrate trisodiums the steps include: with an amount of mass percent concentration to be that being transferred to mass percent concentration with tap water is 38% during 80% phosphoric acid solution is put into and in the still; Be the neutralization of 30% sodium hydroxide solution with an amount of mass percent concentration then,, keep 82 ℃ of temperature of reaction up to neutralizer pH=12.0; The neutralizer that reaction is finished filters, and filtrate is input in the crystallization kettle, when the filtrate temperature reaches 65 ℃, presses 2.5kg/m
3In filtrate, add sodium phosphate, cooling, crystallization is finished, discharging after the crystallization temperature in the kettle drops to 30 ℃, centrifugation, dry, product.
The storage test of the ten phosphate dihydrate trisodiums that make with the present invention.
One, purpose:
Ten phosphate dihydrate trisodium products are done storage test, verify its product stock caking situation.
Two, testing program:
1, sample is packed into 1 kilogram of sample sack, heat-sealing mouthful packing is made 4 bags;
2, above-mentioned 4 product of contracting for fixed output quotas are stacked neatly, put into climatic chamber, temperature is controlled at 50 ℃, and humidity is controlled at 80%, cultivates 120 hours;
3, sample is taken out, observe product caking situation.
4, product appearance does not have the white particle powder of dehydration, does not have hard caking promptly by experiment.
Three, instrument and equipment:
Use the electric heating constant temperature air dry oven, and place two beakers of filling water in baking oven, temperature is controlled at 50 when spending, and humidity is substantially about 80%.
Four, trial sheet:
| Time | Temperature ℃ | Humidity ﹪ | The caking situation |
| The 1st day | 50 | 82 | Do not lump |
| The 2nd day | 50 | 83 | Do not lump |
| The 3rd day | 50 | 80 | Do not lump |
| The 4th day | 50 | 81 | Do not lump |
| The 5th day | 50 | 80 | Do not lump |
Five, conclusion:
After placing 5 days according to the condition in the form in baking oven, take out material and observe, all do not have the white particle powder of dehydration in the product, product is caking not, and product is by test.
Claims (1)
1. the preparation method of hydrophobicity ten phosphate dihydrate trisodiums is characterized in that, the steps include: with an amount of mass percent concentration to be that being transferred to mass percent concentration with tap water is 35 ~ 40% during 75 ~ 85% phosphoric acid solution is put into and in the still; Be the neutralization of 30% sodium hydroxide solution with an amount of mass percent concentration then,, keep 80 ~ 85 ℃ of temperature of reaction up to neutralizer pH=11.5 ~ 12.5; The neutralizer that reaction is finished filters, and filtrate is input in the crystallization kettle, when the filtrate temperature reaches 65 ℃, by 2 ~ 3kg/m
3In filtrate, add sodium phosphate, cooling, crystallization is finished, discharging after the crystallization temperature in the kettle drops to 30 ℃, centrifugation, dry, product.
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| CN 201110173059 CN102259842B (en) | 2011-06-24 | 2011-06-24 | Preparation method of hydrophobic trisodium phosphate dodecahydrate |
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| CN 201110173059 CN102259842B (en) | 2011-06-24 | 2011-06-24 | Preparation method of hydrophobic trisodium phosphate dodecahydrate |
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| CN102259842A true CN102259842A (en) | 2011-11-30 |
| CN102259842B CN102259842B (en) | 2013-01-30 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288067A (en) * | 2013-06-27 | 2013-09-11 | 武汉科梦环境工程有限公司 | Method for recycling phosphates from formed foil pickling wastewater |
| CN104445127A (en) * | 2014-11-27 | 2015-03-25 | 国药集团化学试剂有限公司 | Purifying method of trisodium phosphate |
| CN105133310A (en) * | 2015-09-11 | 2015-12-09 | 无锡市长安曙光手套厂 | Fabric rust remover |
| CN106395777A (en) * | 2016-08-30 | 2017-02-15 | 湖北永绍科技股份有限公司 | Comprehensive utilization method of phosphoric acid waste liquid |
| CN113003554A (en) * | 2021-03-17 | 2021-06-22 | 连云港西都食品配料有限公司 | Preparation method of anhydrous trisodium phosphate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2372282C1 (en) * | 2008-07-04 | 2009-11-10 | Закрытое акционерное общество "Научно-производственная компания "Интерфос" | Method of producing trisodium phosphate |
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2011
- 2011-06-24 CN CN 201110173059 patent/CN102259842B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2372282C1 (en) * | 2008-07-04 | 2009-11-10 | Закрытое акционерное общество "Научно-производственная компания "Интерфос" | Method of producing trisodium phosphate |
Non-Patent Citations (2)
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| 于文锦等: "磷酸三钠的防结块研究", 《无机盐工业》 * |
| 黄培苑: "磷酸三钠的防结块技术研究", 《成都纺织高等专科学校学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288067A (en) * | 2013-06-27 | 2013-09-11 | 武汉科梦环境工程有限公司 | Method for recycling phosphates from formed foil pickling wastewater |
| CN104445127A (en) * | 2014-11-27 | 2015-03-25 | 国药集团化学试剂有限公司 | Purifying method of trisodium phosphate |
| CN104445127B (en) * | 2014-11-27 | 2017-12-12 | 国药集团化学试剂有限公司 | A kind of purification process of tertiary sodium phosphate |
| CN105133310A (en) * | 2015-09-11 | 2015-12-09 | 无锡市长安曙光手套厂 | Fabric rust remover |
| CN106395777A (en) * | 2016-08-30 | 2017-02-15 | 湖北永绍科技股份有限公司 | Comprehensive utilization method of phosphoric acid waste liquid |
| CN113003554A (en) * | 2021-03-17 | 2021-06-22 | 连云港西都食品配料有限公司 | Preparation method of anhydrous trisodium phosphate |
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| CN102259842B (en) | 2013-01-30 |
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Effective date of registration: 20191112 Address after: No.66, Huanghe Road, Donghai Economic Development Zone, Lianyungang City, Jiangsu Province Patentee after: Jiangsu Debang Doling Health Technology Co., Ltd. Address before: 222000 No. 180, new sea road, Haizhou District, Jiangsu, Lianyungang Patentee before: Lianyungang Debang Fine Chemical Co., Ltd. |
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