CN104401958B - A kind of manufacture method of anhydrous chlorides of rase tertiary sodium phosphate - Google Patents
A kind of manufacture method of anhydrous chlorides of rase tertiary sodium phosphate Download PDFInfo
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- CN104401958B CN104401958B CN201410633734.3A CN201410633734A CN104401958B CN 104401958 B CN104401958 B CN 104401958B CN 201410633734 A CN201410633734 A CN 201410633734A CN 104401958 B CN104401958 B CN 104401958B
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- sodium phosphate
- tertiary sodium
- rase
- anhydrous chlorides
- manufacture method
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Abstract
The invention discloses a kind of manufacture method of anhydrous chlorides of rase tertiary sodium phosphate, comprise the following steps: tertiary sodium phosphate, clorox and potassium permanganate are obtained raw mixture according to after the mol ratio Homogeneous phase mixing preset; Add in raw mixture after pure water being preheating to 60 DEG C and make saturated solution, this saturated solution is poured in mixer; Keep the temperature in mixer, saturated solution to be stirred in liquid without after solid, to be sent in crystallizer tank; In crystallizer tank, add additive potassium permanganate, after cooling, obtain crystal; Namely anhydrous chlorides of rase tertiary sodium phosphate is obtained by after crystal filtration, drying.Present invention process flow process is short, and required equipment is simple, less investment, and production cost is lower; Gained Efficacious Disinfeitant good product quality, available chlorine content can reach 4.5%; High-efficiency environment friendly, does not produce toxic waste and waste gas in technological process, without the unmanageable problem of tail gas chloride in traditional technology.
Description
Technical field
The present invention relates to phosphoric acid salt fabricating technology field, particularly relate to a kind of manufacture method of anhydrous chlorides of rase tertiary sodium phosphate.
Background technology
Traditional phosphate product, mentions the anhydrous concept preparing chlorinated sodium phosphate although have, how to be created, and is insurmountable technical problem in industry always, does not also have those skilled in the art to capture at present.
Summary of the invention
Based on this, for existing issue, the invention provides a kind of manufacture method of anhydrous chlorides of rase tertiary sodium phosphate, this technological gap in prior art can be made up.
Technical scheme of the present invention is: a kind of manufacture method of anhydrous chlorides of rase tertiary sodium phosphate, comprises the following steps:
A, by tertiary sodium phosphate, clorox and potassium permanganate according to preset mol ratio Homogeneous phase mixing after obtain raw mixture;
B, pure water is preheating to 60 DEG C after add in raw mixture and make saturated solution, this saturated solution is poured in mixer;
C, the temperature kept in mixer, to be stirred to saturated solution in liquid without after solid, to be sent in crystallizer tank;
D, in crystallizer tank, add additive potassium permanganate, after cooling, obtain crystal;
E, crystal is filtered, namely obtain anhydrous chlorides of rase tertiary sodium phosphate after drying.
In a preferred embodiment, further comprising the steps of: remaining crystalline mother solution after obtained Efficacious Disinfeitant, in sent into salt bath.Object makes remaining crystalline mother solution to obtain recycle.
In a preferred embodiment, in step a, the mol ratio of tertiary sodium phosphate, clorox is 7:3.The anhydrous chlorides of rase tertiary sodium phosphate that such mol ratio obtains best in quality.
In a preferred embodiment, in step b, mixer is electric-type mixer.Object is the convenience being convenient to manufacture.
In a preferred embodiment, in step e, crystal is filtered by whizzer, and adopts vulcanization bed dry.The main effect of whizzer is dehydration, thus saves dry cost; Vulcanization bed drying is also very thorough, is more convenient to carrying out smoothly of whole manufacturing process.
The invention has the beneficial effects as follows:
(1) technical process is short, and required equipment is simple, less investment, and production cost is lower;
(2) gained Efficacious Disinfeitant good product quality, available chlorine content can reach 4.5%;
(3) high-efficiency environment friendly, does not produce toxic waste and waste gas in technological process, without the unmanageable problem of tail gas chloride in traditional technology.
Embodiment
Below embodiments of the invention are described in detail.
Embodiment:
A manufacture method for anhydrous chlorides of rase tertiary sodium phosphate, comprises the following steps:
Step one, obtains raw mixture by tertiary sodium phosphate, clorox and potassium permanganate according to after the mol ratio Homogeneous phase mixing preset; The mol ratio of tertiary sodium phosphate, clorox is 7:3.The anhydrous chlorides of rase tertiary sodium phosphate that such mol ratio obtains best in quality.
Step 2, adds in raw mixture after pure water being preheating to 60 DEG C and makes saturated solution, is poured into by this saturated solution in electric-type mixer;
Step 3, keeps the temperature in mixer, to be stirred to by saturated solution in liquid without after solid, to be sent in crystallizer tank;
Step 4, adds potassium permanganate, obtains crystal after cooling in crystallizer tank;
Step 5, namely obtains anhydrous chlorides of rase tertiary sodium phosphate by after crystal filtration, drying.Remaining crystalline mother solution after obtained Efficacious Disinfeitant, can in be sent into salt bath, can make remaining crystalline mother solution to obtain recycle like this.Crystal is filtered by whizzer, and adopts vulcanization bed dry.The main effect of whizzer is dehydration, thus saves dry cost; Vulcanization bed drying is also very thorough, is more convenient to carrying out smoothly of whole manufacturing process.
Technical process of the present invention is short, and required equipment is simple, less investment, and production cost is lower; Gained Efficacious Disinfeitant good product quality, available chlorine content can reach 4.5%; High-efficiency environment friendly, does not produce toxic waste and waste gas in technological process, without the unmanageable problem of tail gas chloride in traditional technology.
Experiment parameter is analyzed:
1, solution reaction parameter
The experiment parameter of Na:P: select .CNa/CP2.7:1 in sodium phosphate salt batching to be advisable, now in batching, the mol ratio of Na3PO3 and Na2HPO is 7:3.
2, temperature of reaction experiment parameter:
Temperature is higher than after 70 degree, and NaOCl content is high, and Na3PO4 content also meets the requirements, and synthesis temperature controls at 60-80.
3, drying time controls
4, proportioning raw materials and the experiment of synthesis top condition reproducibility
Below experiment parameter illustrates:
(1) proportioning raw materials: excessive based on NaOCl;
(2) Reactive Synthesis temperature is based on 60-70;
(3) drying temperature controls at 30 degree is main;
(4) production quality control is mainly at batching mode, temperature control, the type of cooling, the reaction of feed way under temperature controls.
Adopt the anhydrous chlorides of rase sodium phosphate that above manufacture technics goes out, there is following characteristic:
1, molecular formula is: 4 (Na
3pO
4.11H
2o) .NaOCl; Also can be: Cl – TSP;
2, color is: pink or white;
3, index is: pH value (1%solution): 11.6-12.0;
4、B.D.(pouring)gm/cc:0.75；
5, moisture content (at110 DEG C): 44.0-47.5;
6, water-insoluble: 0.05%;
7、P
2O
5:17.5-19.5％；
8, fuel value: 45.0-49.0;
9, iron ion: 50.0PPM;
10, active phosphorus: 3.5.
Constant product quality, chloride content is stablized, without the three wastes.
The above embodiment only have expressed the specific embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.
Claims (5)
1. a manufacture method for anhydrous chlorides of rase tertiary sodium phosphate, is characterized in that, comprises the following steps:
A, by tertiary sodium phosphate, clorox and potassium permanganate according to preset mol ratio Homogeneous phase mixing after obtain raw mixture;
B, pure water is preheating to 60 DEG C after add in raw mixture and make saturated solution, this saturated solution is poured in mixer;
C, the temperature kept in mixer, to be stirred to saturated solution in liquid without after solid, to be sent in crystallizer tank;
D, in crystallizer tank, add additive potassium permanganate, after cooling, obtain crystal;
E, crystal is filtered, namely obtain anhydrous chlorides of rase tertiary sodium phosphate after drying.
2. the manufacture method of anhydrous chlorides of rase tertiary sodium phosphate according to claim 1, is characterized in that, further comprising the steps of:
Remaining crystalline mother solution after obtained Efficacious Disinfeitant, in sent into salt bath.
3. the manufacture method of anhydrous chlorides of rase tertiary sodium phosphate according to claim 1 and 2, is characterized in that, in step a, the mol ratio of tertiary sodium phosphate, clorox is 7:3.
4. the manufacture method of anhydrous chlorides of rase tertiary sodium phosphate according to claim 1 and 2, is characterized in that, in step b, mixer is electric-type mixer.
5. the manufacture method of anhydrous chlorides of rase tertiary sodium phosphate according to claim 1 and 2, is characterized in that, in step e, crystal is filtered by whizzer, and adopts vulcanization bed dry.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410633734.3A CN104401958B (en) | 2014-11-12 | 2014-11-12 | A kind of manufacture method of anhydrous chlorides of rase tertiary sodium phosphate |
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| CN201410633734.3A CN104401958B (en) | 2014-11-12 | 2014-11-12 | A kind of manufacture method of anhydrous chlorides of rase tertiary sodium phosphate |
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| CN104401958A CN104401958A (en) | 2015-03-11 |
| CN104401958B true CN104401958B (en) | 2016-02-24 |
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| CN201410633734.3A Expired - Fee Related CN104401958B (en) | 2014-11-12 | 2014-11-12 | A kind of manufacture method of anhydrous chlorides of rase tertiary sodium phosphate |
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| CN111001183A (en) * | 2019-09-09 | 2020-04-14 | 湖南中核金原新材料有限责任公司 | Double-effect continuous crystallization method of trisodium phosphate |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3525583A (en) * | 1965-09-01 | 1970-08-25 | Diversey Corp | Process for producing the complex,(na3po411h2o)4 naclo |
| US3551094A (en) * | 1967-11-28 | 1970-12-29 | Olin Corp | Process for producing non-caking chlorinated trisodium phosphate |
| US3656890A (en) * | 1969-09-05 | 1972-04-18 | Stouffer Chemical Co | Chlorinated trisodium phosphates |
| US4402926A (en) * | 1981-09-28 | 1983-09-06 | Monsanto Company | Process for producing chlorinated trisodium phosphate |
| SU1100229A1 (en) * | 1982-03-23 | 1984-06-30 | Предприятие П/Я А-7346 | Method for producing chlorinated trisodium phosphate |
| CN103420351A (en) * | 2013-08-06 | 2013-12-04 | 贵州开磷（集团）有限责任公司 | Preparation technology for chlorinated trisodium phosphate |
-
2014
- 2014-11-12 CN CN201410633734.3A patent/CN104401958B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3525583A (en) * | 1965-09-01 | 1970-08-25 | Diversey Corp | Process for producing the complex,(na3po411h2o)4 naclo |
| US3551094A (en) * | 1967-11-28 | 1970-12-29 | Olin Corp | Process for producing non-caking chlorinated trisodium phosphate |
| US3656890A (en) * | 1969-09-05 | 1972-04-18 | Stouffer Chemical Co | Chlorinated trisodium phosphates |
| US4402926A (en) * | 1981-09-28 | 1983-09-06 | Monsanto Company | Process for producing chlorinated trisodium phosphate |
| SU1100229A1 (en) * | 1982-03-23 | 1984-06-30 | Предприятие П/Я А-7346 | Method for producing chlorinated trisodium phosphate |
| CN103420351A (en) * | 2013-08-06 | 2013-12-04 | 贵州开磷（集团）有限责任公司 | Preparation technology for chlorinated trisodium phosphate |
Non-Patent Citations (3)
| Title |
|---|
| 合成氯化磷酸三钠的实验研究;董桂英;《中国氯碱》;20021130;第22-23页 * |
| 改进氯化磷酸三钠的生产工艺研究;周玉新等;《武汉化工学院学报》;19951231;第17卷(第4期);第24-27页 * |
| 氯化磷酸三钠生产新工艺研究;肖德良等;《湖北化工》;19931231;第42-44页 * |
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