CN104876232A - Method for preparing active calcium silicate by using phosphorus gypsum - Google Patents
Method for preparing active calcium silicate by using phosphorus gypsum Download PDFInfo
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- CN104876232A CN104876232A CN201510256926.1A CN201510256926A CN104876232A CN 104876232 A CN104876232 A CN 104876232A CN 201510256926 A CN201510256926 A CN 201510256926A CN 104876232 A CN104876232 A CN 104876232A
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- phosphogypsum
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Abstract
The invention discloses a method for preparing active calcium silicate by using phosphorus gypsum. The method for preparing the active calcium silicate by using phosphorus gypsum comprises the following steps: preprocessing the phosphorus gypsum which serves as the raw material and is a side product in the process of producing phosphoric acid through a wet process, reacting, synthesizing, filtering and activating. By virtue of the method, a large amount of phosphorus gypsum is consumed for preparing active calcium silicate products which are relatively high in additional values, so that a certain economic benefit is created; the problem of the treatment on phosphorus gypsum solid waste with influence on the development of the phosphorus chemical industry for a long time can also be solved; the waste is changed into wealth. The produced calcium silicate products are high in activity and excellent in adsorption performance and reinforcement performance, and can be widely used in papermaking, rubber, plastic industries as fillers.
Description
Technical field
The present invention relates to a kind of method utilizing phosphogypsum to prepare active calcium silicate, belong to phosphorous chemical industry field.
Background technology
Active calcium silicate, also known as making polymolecularity Calucium Silicate powder, is a kind of new silicate product.Because granularity is superfine, being 20-50 micron, there is the siloxy identical with white carbon black and silanol base functional group in surface, there is very strong reinforcing property, under same equigranular, its reinforcing function is suitable with white carbon black, but its production cost is at half than white carbon black, can be used to replace white carbon black.Industrial active calcium silicate, except a large amount of strengthening agent for rubber, plastics, is all used widely as raw material and additive at the industrial sector such as papermaking, coating (papermaking paint and chemistry painting industry), medicine, ink, agricultural chemicals.
The preparation method of current active calcium silicate is mainly hydrothermal synthesis method, reacts preparation under certain condition and obtain with certain density calcium salt and aqueous silicate solution.Application number be 200810068999.8 national patent " a kind of Calucium Silicate powder and preparation method thereof " disclose a kind of preparation method of Calucium Silicate powder, industrial calcium chloride and industrial metasilicate is utilized to be raw material, by adding coagent, calcium silicate products is prepared after the techniques such as purification, removal of impurities, although this method processing step is simple, but the higher and product of raw materials used cost is mainly used as the integral part of the slag in molten silicon, and added value of product is low; Application number be 2013100007024.5 national patent " a kind of preparation method of active calcium silicate " disclose a kind of production method of active calcium silicate, be that raw material collects the limestone particle of below granularity 10mm through treatment process such as calcining, cooling, screenings with Wingdale, and carry out ashing treatment and make milk of lime, react with sodium silicate solution and prepare active calcium silicate, there is the shortcomings such as cost is higher equally in this method, simultaneously due to without activation treatment, active poor, product is used as industrial filler mostly.
Summary of the invention
The object of the invention is to overcome above-mentioned shortcoming, a kind of method preparing active calcium silicate that raw materials cost is low, Product Activity is high is provided.
Technical scheme of the present invention is: a kind of method utilizing phosphogypsum to prepare active calcium silicate, mainly be divided into 4 processing steps: 1. raw materials pretreatment: get a certain amount of phosphogypsum, add the water (water: phosphogypsum) that mass ratio is 1 ~ 3:1 and make mixing solutions, controlling solution temperature is 70 ~ 90 DEG C, and stirring velocity 300rpm, slowly adds lime powder, pH is made to be 7 ~ 9, after reaction 1 ~ 2h, filtered by solution, filter cake uses 200g water washing three times at every turn.
2. Reactive Synthesis: get a certain amount of through above-mentioned pretreated phosphogypsum, add certain water gaging and make the mixing solutions that solid content is 50%, slowly add the sodium silicate solution that mass concentration mark is 10% ~ 40% wherein, control temperature of reaction 70 ~ 90 DEG C, stirring velocity 200 ~ 400rpm, reaction times 1 ~ 3h, water glass are 1 ~ 1.4:1 with phosphogypsum quality ratio;
3. filtering: by above-mentioned reacting liquid filtering after Reactive Synthesis step, filter cake washes with water, is till 7 ~ 8 until pH;
4. activate: get the filter cake in above-mentioned filtration step technique, be placed in retort furnace, control temperature is 600 ~ 700 DEG C, activation 1 ~ 2h, obtains Product Activity Calucium Silicate powder.
The mass concentration of sodium silicate solution used is 10% ~ 40%; The elementary composition of phosphogypsum used is calcium sulfate 80%-85%, phosphatase 11 %-2%, sulfuric acid 0.04%-0.2%, and surplus is water.
Active calcium silicate preparation method of the present invention adopts cheap phosphogypsum as raw material, in retort furnace, obtain active high calcium silicate products through high-temperature activation simultaneously, can use as raw material and additive at the industrial sector such as papermaking, coating (papermaking paint and chemistry painting industry), medicine, ink, agricultural chemicals.
Embodiment
embodiment 1
Get 200g phosphogypsum, add 200g water, under temperature 70 C, stirring velocity 300rpm condition, slowly add lime powder, pH is filtered after 8,1h, and filter cake uses 100g water washing three times at every turn.Learn from else's experience the filter cake 100g after above-mentioned process, add 100g water and make mixing solutions, slowly add the sodium silicate solution 1000g altogether that mass concentration is 10%, control temperature of reaction 70 DEG C, stirring velocity 200rpm, reaction times 1h, reaction terminates rear filtration, and it is 7 ~ 8 that filter cake is washed with distilled water to pH, after having washed, filter cake is placed in retort furnace, control temperature is 600 DEG C, soak time is 1h, obtains Product Activity Calucium Silicate powder.CaO content 46.09%, SiO in product after testing
2content 52.33%.
embodiment 2
Get 200g phosphogypsum, add 600g water, under temperature 90 DEG C, stirring velocity 300rpm condition, slowly add lime powder, pH is filtered after 9,2h, and filter cake uses 100g water washing three times at every turn.Learn from else's experience the filter cake 100g after above-mentioned process, add 100g water and make mixing solutions, slowly add the sodium silicate solution 350g altogether that mass concentration is 40%, control temperature of reaction 90 DEG C, stirring velocity 400rpm, reaction times 3h, reaction terminates rear filtration, and it is 7 ~ 8 that filter cake is washed with distilled water to pH, after having washed, filter cake is placed in retort furnace, control temperature is 700 DEG C, soak time is 1h, obtains Product Activity Calucium Silicate powder.CaO content 47.28%, SiO in product after testing
2content 51.46%.
embodiment 3
Get 200g phosphogypsum, add 400g water, under temperature 80 DEG C, stirring velocity 300rpm condition, slowly add lime powder, pH is filtered after 8,1h, and filter cake uses 100g water washing three times at every turn.Learn from else's experience the filter cake 100g after above-mentioned process, add 100g water and make mixing solutions, slowly add the sodium silicate solution 600g altogether that mass concentration is 20%, control temperature of reaction 80 DEG C, stirring velocity 300rpm, reaction times 2h, reaction terminates rear filtration, and it is 7 ~ 8 that filter cake is washed with distilled water to pH, after having washed, filter cake is placed in retort furnace, control temperature is 600 DEG C, soak time is 2h, obtains Product Activity Calucium Silicate powder.CaO content 46.54%, SiO in product after testing
2content 52.17%.
embodiment 4
Get 200g phosphogypsum, add 300g water, under temperature 70 C, stirring velocity 300rpm condition, slowly add lime powder, pH is filtered after 9,1h, and filter cake uses 100g water washing three times at every turn.Learn from else's experience the filter cake 100g after above-mentioned process, add 100g water and make mixing solutions, slowly add the sodium silicate solution 433g altogether that mass concentration is 30%, control temperature of reaction 80 DEG C, stirring velocity 200rpm, reaction times 2h, reaction terminates rear filtration, and it is 7 ~ 8 that filter cake is washed with distilled water to pH, after having washed, filter cake is placed in retort furnace, control temperature is 700 DEG C, soak time is 2h, obtains Product Activity Calucium Silicate powder.CaO content 47.01%, SiO in product after testing
2content 51.5%.
Claims (2)
1. the method utilizing phosphogypsum to prepare active calcium silicate, it is characterized in that mainly being divided into 4 processing steps: 1. raw materials pretreatment: get a certain amount of phosphogypsum, add quality than water: phosphogypsum is that the water of 1 ~ 3:1 makes mixing solutions, controlling solution temperature is 70 ~ 90 DEG C, and stirring velocity 300rpm, slowly adds lime powder, pH is made to be 7 ~ 9, after reaction 1 ~ 2h, filtered by solution, filter cake uses 200g water washing three times at every turn;
2. Reactive Synthesis: get a certain amount of through above-mentioned pretreated phosphogypsum, add certain water gaging and make the mixing solutions that solid content is 50%, slowly add the sodium silicate solution that mass concentration mark is 10% ~ 40% wherein, control temperature of reaction 70 ~ 90 DEG C, stirring velocity 200 ~ 400rpm, reaction times 1 ~ 3h, water glass are 1 ~ 1.4:1 with phosphogypsum quality ratio;
3. filtering: by above-mentioned reacting liquid filtering after Reactive Synthesis step, filter cake washes with water, is till 7 ~ 8 until pH;
4. activate: get the filter cake in above-mentioned filtration step technique, be placed in retort furnace, control temperature is 600 ~ 700 DEG C, activation 1 ~ 2h, obtains Product Activity Calucium Silicate powder.
2. the method utilizing phosphogypsum to prepare active calcium silicate according to claim 1, is characterized in that the mass concentration of sodium silicate solution used is 10% ~ 40%; The elementary composition of phosphogypsum used is calcium sulfate 80%-85%, phosphatase 11 %-2%, sulfuric acid 0.04%-0.2%, and surplus is water.
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| CN201510256926.1A CN104876232A (en) | 2015-05-20 | 2015-05-20 | Method for preparing active calcium silicate by using phosphorus gypsum |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731475A (en) * | 2016-01-27 | 2016-07-06 | 河南王屋纳米科技有限责任公司 | Preparation method of calcium silicate powder with low pH value, high oil absorption value and large specific surface area |
| CN108165029A (en) * | 2018-02-11 | 2018-06-15 | 贵州开磷磷石膏综合利用有限公司 | A kind of micronization modified method of ardealite as PVC fillers |
| CN114349570A (en) * | 2022-02-11 | 2022-04-15 | 瓮福（集团）有限责任公司 | Preparation method of calcium silicon fertilizer |
| CN115814750A (en) * | 2022-12-15 | 2023-03-21 | 贵州大学 | Method for preparing porous calcium silicate adsorbent from phosphogypsum |
-
2015
- 2015-05-20 CN CN201510256926.1A patent/CN104876232A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731475A (en) * | 2016-01-27 | 2016-07-06 | 河南王屋纳米科技有限责任公司 | Preparation method of calcium silicate powder with low pH value, high oil absorption value and large specific surface area |
| CN108165029A (en) * | 2018-02-11 | 2018-06-15 | 贵州开磷磷石膏综合利用有限公司 | A kind of micronization modified method of ardealite as PVC fillers |
| CN114349570A (en) * | 2022-02-11 | 2022-04-15 | 瓮福（集团）有限责任公司 | Preparation method of calcium silicon fertilizer |
| CN115814750A (en) * | 2022-12-15 | 2023-03-21 | 贵州大学 | Method for preparing porous calcium silicate adsorbent from phosphogypsum |
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Application publication date: 20150902 |