CN1278512A - Production process of fine active calcium phosphate - Google Patents
Production process of fine active calcium phosphate Download PDFInfo
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- CN1278512A CN1278512A CN 00109945 CN00109945A CN1278512A CN 1278512 A CN1278512 A CN 1278512A CN 00109945 CN00109945 CN 00109945 CN 00109945 A CN00109945 A CN 00109945A CN 1278512 A CN1278512 A CN 1278512A
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- calcium phosphate
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Abstract
The production method of microfine active calcium phosphate includes the following steps: making calcium hydroxide and phosphoric acid implement neutralization reaction in water, adding proper quantity of sodium dodecylbenzenesulfonate as dispersion aid and using sodium pyrophosphate as corrosion inhibitor to obtain an emulsion-like material, then making said emulsion-like material undergo the processes of monitoring, press-filtering, washing, spray-drying, grinding to make powder and seiving to obtain the invented microfine powder product with 400 meshes. It can be used as dispersing agent for suspension polymerization of resins of SAN, PS, EPS, GPPS and HIPS, etc., can be used as parting agent for adhesion prevention of resin, as clarifying agent in sugar industry and demoulding agent in metal casting industry, etc.. It possesses extensive application range, and is favorable for large-scole industrial production.
Description
The present invention relates to the improvement of active calcium phosphate production method, particularly a kind of production method of superfine active calcium phosphate is applicable to that resins such as suspension polymerization SAN, PS, EPS, GPPS, HIPS make dispersion agent.Also can make the antiseized separant of resin, the heavy clear agent of sugar industry, the releasing agent in the metal casting all is widely used at aspects such as optics, dentistry, bone material, ion exchange resin.
Active calcium phosphate (HAP or TCP) belongs to hydroxy kind, has another name called calcium phosphate powder, it is a kind of water-insoluble inorganic dispersant, this inorganic dispersant is compared with water-soluble polymer (as polyvinyl alcohol) dispersion agent, especially on suspension polymerization coarse grain PS, many advantages are arranged, there is special effect the outward appearance and the production efficiency that improve rosin products, aspect such as reduce cost, and it occupies critical role in plastics industry.The patent of invention specification sheets of publishing according to Patent Office of the People's Republic of China (CN103521C) is called the active calcium phosphate that " production technology of active calcium phosphate " patent is produced, though many advantages are arranged as specification sheets is said, but still have its limitation: as its product as described in the specification sheets is the emulsus material, promptly is not easy to transportation, only is suitable for small-sized production; In the half sedimentation cycle of not strict control emulsus material in the production process, will be difficult to reach suspension polymerization and make the effect of dispersion agent (because of half sedimentation cycle was the active rerum natura characteristic index of proof HAP); Its Cl of HAP without washing
-Impurity such as ion are sneaked into the quality that will influence production high-clarity polymer resin in the dispersion system; Do not add SDBS (Sodium dodecylbenzene sulfonate) dispersion aids, will reduce greatly during polymerization the monomer droplet surface adsorption rate, and can lump.
Purpose of the present invention is exactly in order to overcome above-mentioned the deficiencies in the prior art part, and production technique is improved, gone out a kind of fine active calcium phosphate with production method direct production of the present invention.
The objective of the invention is to realize in following mode: comprise composition of raw materials (by weight): 100 parts in water, calcium hydroxide 6-9 part, phosphatase 24-8 part, trisodium phosphate add in the ratio of the 0.2-1.2% of phosphoric acid weight, and it is undertaken by following step successively:
(1) purified milk of lime is mixed with the Ca (OH) of 6-15%
2The aqueous solution, put into reactor and stir, intensification 50-80 ℃,
(2) phosphorylated ligand is made the aqueous solution of 40-50%, be added dropwise in the reactor, the neutralization reaction temperature is controlled at 50-80 ℃, and the reaction end pH value is controlled at 6-9, after reaction times 2-3 hour, the emulsus material, it is characterized in that:
(3) half sedimentation cycle t of monitoring emulsus material
1/2＞10min,
(4) carry out press filtration, washing except that Cl
-Impurity such as ion,
(5) change dosing chamber over to, control solid substance＞15%, and press solid substance weight ground 20 * 10
-6-100 * 10
-6Ratio add dispersion aids SDBS, stir 30min,
(6) enter spray-drying tower, when the spray-drying tower inlet temperature reaches 250 ℃, when temperature out reaches 150 ℃, then carries out the material spray drying,
(7) dried feed enter grinding, again through the screening, fineness＞400 orders promptly gets ultrafine powder powder product.
Product of the present invention is that powder-material, fineness reach more than 400 orders.It is just more stable because of the inorganic dispersant particle is healed carefully, then the area coverage of certain consumption is bigger, suspension is joined by institute.Half sedimentation cycle also was the index of the stability of evaluation dispersion liquid, so need monitoring.When HAP makes dispersion agent, add an amount of Sodium dodecylbenzene sulfonate (SDBS) and make buffer reagent with trisodium phosphate, has specific effect, further reduced interfacial tension on the one hand, tensio-active agent can change the characteristic of HAP powder again on the other hand, increase its lipophilicity and adsorptive capacity, improve the utilization ratio of powder, the adsorptive capacity on monomer whose drop surface will improve 6-7 doubly.As, HAP is not about 9.8% in the adsorption rate on vinylbenzene drop surface when adding SDBS, will lump during polymerization; Adsorption rate increases to 65.8% behind an amount of SDBS, polymerization system is also stable simultaneously and add.And SDBS adds with the raw material of preparation during HAP can obtain good result.Product of the present invention can be packed with Polywoven Bag, is convenient to transportation, helps large-scale commercial production.
Describe in detail below in conjunction with accompanying drawing.
Accompanying drawing is a process flow diagram of the present invention.
Embodiment one: composition of raw materials (by weight) is as follows:
100 parts in water
6 parts in calcium hydroxide
Phosphatase 24 part
0.008 part of trisodium phosphate
Referring to accompanying drawing, undertaken by 1-9 step among the figure:
(1) with the aqueous solution of the calcium hydroxide of purified milk of lime preparation 6%, put into reactor and stir, be warmed up to 50 ℃ (1-2 steps among the figure),
(2) phosphorylated ligand is made 40% the aqueous solution, be added dropwise in the reactor, the neutralization reaction temperature is controlled at 50 ℃, and the reaction end pH value is controlled at 6,2 hours reaction times, emulsus material (the 3rd step among the figure), its reaction equation is as follows:
(3) half sedimentation cycle t of monitoring emulsus material
1/2＞10min,
(4) carry out press filtration, washing except that Cl
-Impurity such as ion (the 4th step among the figure)
(5) change over to and join stock tank, control solid substance＞15%, and press 20 * 10 of solid substance weight
-6Ratio add dispersion aids SDBS, stir 12min (the 5th step among the figure)
(6) enter spray-drying tower, when the spray-drying tower inlet temperature reaches 250 ℃, when temperature out reaches 150 ℃, then carries out material spray drying (the 6th step among the figure)
(7) dry mash enter grinding, again through screening (among the figure the 7th, 8 step), when fineness＞400 orders, then fines shape HAP product, enter product storage tank (the 9th step finished among the figure).
Embodiment two: composition of raw materials (by weight):
100 parts in water
7 parts in calcium hydroxide
5 parts of phosphoric acid
0.035 part of trisodium phosphate
Carry out according to the following steps:
(1) purified milk of lime is mixed with the aqueous solution of 8% calcium hydroxide, puts into reactor and stir, be warming up to 60 ℃,
(2) phosphorylated ligand is made 42% the aqueous solution, be added dropwise in the reactor, the neutralization reaction temperature is controlled at 60 ℃, and the reaction end pH value is controlled at 7, after 2 hours reaction times, the emulsus material, behind monitoring step and press filtration, washing step,
(3) change over to and join stock tank, solid substance＞15%, and press 40 * 10 of solid substance weight
-6Ratio add dispersion aids SDBS, stir 20min.
All the other technical requirementss are with embodiment one.
Embodiment three: composition of raw materials (by weight):
100 parts in water
7.5 parts in calcium hydroxide
6 parts of phosphoric acid
0.042 part of trisodium phosphate
Carry out according to the following steps:
(1) purified milk of lime is mixed with the aqueous solution of 10% calcium hydroxide, puts into reactor and stir, and be warming up to 70 ℃,
(2) phosphorylated ligand is made 45% the aqueous solution, be added dropwise in the reactor, the neutralization reaction temperature is controlled at 70 ℃, and the reaction end pH value is controlled at 8,2.5 hours reaction times, behind the emulsus material, undertaken by monitoring and press filtration, washing step,
(3) change over to and join stock tank, still control solid substance＞15%, and press 70 * 10 of solid substance weight
-6Ratio add dispersion aids SDBS, stir 28min.
All the other are with embodiment one.
Embodiment four: composition of raw materials (by weight):
100 parts in water
9 parts in calcium hydroxide
8 parts of phosphoric acid
0.096 part of trisodium phosphate
Carry out according to the following steps:
(1) purified milk of lime is mixed with 5% the aqueous solution, puts into reactor and stir, be warming up to 80 ℃,
(2) phosphorylated ligand is made 50% the aqueous solution, is added dropwise in the reactor, 80 ℃ of neutralization reaction temperature, the reaction end pH value is controlled at 9,3 hours reaction times, behind the emulsus material, after being undertaken by monitoring step and press filtration, washing step, enter:
(3) join stock tank, still control solid substance＞15%, and press 100 * 10 of solid substance weight
-6Ratio add and to help branch agent SDBS, stir 30min.
All the other make fines shape HAP product with embodiment one technical requirements.
Claims (2)
1, a kind of production method of fine active calcium phosphate, comprise composition of raw materials (by weight): 100 parts in water, 6～9 parts in calcium hydroxide, phosphatase 24～8 part, trisodium phosphate add in 0.2～1.2% ratio of phosphoric acid weight, and it is undertaken by following step successively:
(1) purified milk of lime is mixed with the Ca (OH) of 6-15%
2The aqueous solution, put into reactor and stir, intensification 50-80 ℃,
(2) phosphorylated ligand is made the aqueous solution of 40-50%, be added dropwise in the reactor, the neutralization reaction temperature is controlled at 50-80 ℃, and reaction end PH is controlled at 6-9, after reaction times 2-3 hour, the emulsus material, it is characterized in that:
(3) half sedimentation cycle t of monitoring emulsus material
1/2＞10min,
(4) carry out press filtration, washing except that Cl
-Impurity such as ion,
(5) change dosing chamber over to, control solid substance＞15%, and press 20 * 10 of solid substance weight
-6---100 * 10
-6Ratio add dispersion aids SDBS, stir 30min,
(6) enter spray-drying tower, when the spray-drying tower inlet temperature reaches 250 ℃, when temperature out reaches 150 ℃, then carries out the material spray drying,
(7) dried feed enter grinding, again through the screening, fineness＞400 orders promptly gets ultrafine powder powder product.
2, the production method of fine active calcium phosphate according to claim 1 is characterized in that: described buffer reagent trisodium phosphate and dispersion aids Sodium dodecylbenzene sulfonate (SDBS) add when preparation of raw material together in proportion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001099450A CN1133579C (en) | 2000-07-25 | 2000-07-25 | Production process of fine active calcium phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001099450A CN1133579C (en) | 2000-07-25 | 2000-07-25 | Production process of fine active calcium phosphate |
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| Publication Number | Publication Date |
|---|---|
| CN1278512A true CN1278512A (en) | 2001-01-03 |
| CN1133579C CN1133579C (en) | 2004-01-07 |
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|---|---|---|---|
| CNB001099450A Expired - Fee Related CN1133579C (en) | 2000-07-25 | 2000-07-25 | Production process of fine active calcium phosphate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101905133A (en) * | 2010-06-28 | 2010-12-08 | 四川绵竹川润化工有限公司 | Novel active calcium phosphate and preparation method thereof |
| CN101423205B (en) * | 2008-11-25 | 2011-03-16 | 邓旭亮 | Synthesis technique of beta-calcium orthophosphate |
| CN103979511A (en) * | 2014-05-15 | 2014-08-13 | 连云港格兰特化工有限公司 | Continuously operable active calcium phosphate production method |
| CN115636399A (en) * | 2022-09-08 | 2023-01-24 | 昆明川金诺化工股份有限公司 | Production process of active calcium phosphate with high activity and stable quality |
-
2000
- 2000-07-25 CN CNB001099450A patent/CN1133579C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423205B (en) * | 2008-11-25 | 2011-03-16 | 邓旭亮 | Synthesis technique of beta-calcium orthophosphate |
| CN101905133A (en) * | 2010-06-28 | 2010-12-08 | 四川绵竹川润化工有限公司 | Novel active calcium phosphate and preparation method thereof |
| CN101905133B (en) * | 2010-06-28 | 2012-06-27 | 四川绵竹川润化工有限公司 | Novel active calcium phosphate and preparation method thereof |
| CN103979511A (en) * | 2014-05-15 | 2014-08-13 | 连云港格兰特化工有限公司 | Continuously operable active calcium phosphate production method |
| CN103979511B (en) * | 2014-05-15 | 2016-03-09 | 连云港格兰特化工有限公司 | A kind of can the active calcium phosphate production method of operate continuously |
| CN115636399A (en) * | 2022-09-08 | 2023-01-24 | 昆明川金诺化工股份有限公司 | Production process of active calcium phosphate with high activity and stable quality |
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| Publication number | Publication date |
|---|---|
| CN1133579C (en) | 2004-01-07 |
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