CN113133949A - Production method of sodium trimetaphosphate as abrasive for toothpaste - Google Patents

Production method of sodium trimetaphosphate as abrasive for toothpaste Download PDF

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Publication number
CN113133949A
CN113133949A CN202110494256.2A CN202110494256A CN113133949A CN 113133949 A CN113133949 A CN 113133949A CN 202110494256 A CN202110494256 A CN 202110494256A CN 113133949 A CN113133949 A CN 113133949A
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CN
China
Prior art keywords
toothpaste
sodium
sodium trimetaphosphate
abrasive
dihydrogen phosphate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110494256.2A
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Chinese (zh)
Inventor
戴中超
田大林
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Lianyungang Xidu Food Ingredients Co Ltd
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Lianyungang Xidu Food Ingredients Co Ltd
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Priority to CN202110494256.2A priority Critical patent/CN113133949A/en
Publication of CN113133949A publication Critical patent/CN113133949A/en
Pending legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/24Phosphorous; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/38Condensed phosphates
    • C01B25/44Metaphosphates
    • C01B25/445Metaphosphates of alkali metals
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/28Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Public Health (AREA)
  • Organic Chemistry (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Veterinary Medicine (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Cosmetics (AREA)

Abstract

A method for producing sodium trimetaphosphate used as an abrasive for toothpaste comprises the following steps: adding phosphoric acid into a reaction kettle, stirring, adding sodium salt, detecting the pH value to be 3.0-4.5 on line, heating for reaction, and after the reaction is finished, crystallizing, performing spin filtration, drying and crushing to obtain the anhydrous sodium dihydrogen phosphate particles. And calcining the sodium dihydrogen phosphate particles twice, crushing and sieving to obtain the sodium trimetaphosphate for the toothpaste. The method has simple process, and improves the purity of the sodium dihydrogen phosphate by adopting the steps of online pH monitoring, crystallization, ethanol washing and the like in the process of producing the sodium dihydrogen phosphate. Inert gas is filled in the sodium dihydrogen phosphate calcination process, and the modes of slow temperature reduction and crushing are adopted, so that the purity of the sodium trimetaphosphate is ensured, and solid caking and the like are reduced. The sodium trimetaphosphate obtained by the method has high purity and fine particles, and can ensure the quality of toothpaste abrasive.

Description

Production method of sodium trimetaphosphate as abrasive for toothpaste
Technical Field
The invention relates to a production method of a toothpaste abrasive, in particular to a method for taking sodium trimetaphosphate as an abrasive.
Background
Toothpaste is a cleaning product for people in modern society. The types of the toothpaste have single cleaning type and are developed into multifunctional types with various functions and complete varieties. The toothpaste abradant is used for rubbing teeth to remove stains during tooth brushing, so that the teeth are whitened, and the toothpaste abradant accounts for about 40-50% of the toothpaste. The currently used toothpaste abrasives include silicon dioxide, calcium carbonate, calcium hydrogen phosphate and the like, and the principle is that after the granular abrasives are repeatedly rubbed on the surfaces of teeth, food residues attached to the surfaces of the teeth are removed, so that the teeth are cleaned. However, since these abrasives are mostly insoluble or slightly water-soluble particles, their hardness is high, and long-term rubbing may destroy the smoothness of the tooth surface, cause tooth discoloration and erosion, and cause some damage to teeth.
Sodium trimetaphosphate has higher washing performance due to the hexahydric cyclic molecular structure. Sodium trimetaphosphate is used as a toothpaste abrasive, and calcium, magnesium, titanium and other ions on teeth generate a relatively strong soluble complex compound according to the principle, so that a softer abrasive is formed, and smoke stains, tea stains and the like on the teeth are removed. Sodium trimetaphosphate complexes calcium in rusty stains on teeth to achieve the effect of slowly removing stains. Sodium trimetaphosphate also has the functions of preventing and removing dental caries. Because the texture is soft, the tooth glaze surface can not be damaged, the water-holding and stabilizing performance is good, the dosage of the adhesive and the wetting agent can be reduced, and the cost is reduced.
The invention content is as follows: aiming at the defects of the prior art, the invention provides a method for producing toothpaste abradant by using sodium trimetaphosphate, which comprises the following steps,
the method comprises the following steps: adding phosphoric acid solution into a reaction kettle, stirring, slowly adding sodium salt, detecting the pH range to be 3.0-4.5 on line, heating to 40-60 ℃, and reacting for 2-3 hours. And after the reaction is finished, crystallizing, cooling to 0-10 ℃ while stirring, stirring for 2-3 hours, adding the reaction liquid into a centrifugal machine, throwing and filtering until no liquid flows out, adding ethanol into the centrifugal machine, continuing throwing and filtering, collecting filter cakes after no liquid flows out, putting the filter cakes into an oven, setting the temperature to be 60-70 ℃, and drying for 4-5 hours to obtain the anhydrous sodium dihydrogen phosphate. Pulverizing in pulverizer to obtain anhydrous sodium dihydrogen phosphate granule with purity of 98.5-99.8%.
Step two: adding anhydrous sodium dihydrogen phosphate particles into a crucible, filling inert gas, heating to the temperature of 200-240 ℃, calcining for 3-4 hours, and finishing the reaction. Slowly cooling to room temperature, and pulverizing into granules with a pulverizer. And putting the mixture into the crucible again, filling inert gas, heating the mixture to the temperature of 560 ℃ and 600 ℃, and continuing calcining the mixture for 5 to 7 hours. And cooling to room temperature to obtain sodium trimetaphosphate solid.
Step three: and (3) crushing the solid sodium trimetaphosphate by using a crusher, and screening particles by using a screen to obtain the sodium trimetaphosphate as the abrasive for the toothpaste.
Further, the sodium salt used in the first step is sodium hydroxide, sodium bicarbonate or sodium carbonate.
Further, the centrifuge used in the first step is an antiseptic centrifuge.
Further, the concentration of the ethanol used in the first step is 90-95%.
Further, the step one oven is a blast oven.
Furthermore, the crucible used in the second step is a closed type.
Further, the inert gas used in the second step is nitrogen or helium.
Further, the pulverizer used in the second step is a jet mill.
Furthermore, the aperture of the brush used in the second step is 5-10 μm.
The toothpaste uses sodium trimetaphosphate as an abrasive production method, controls the end point of sodium dihydrogen phosphate reaction by monitoring pH on line, and uses ethanol solution to remove excessive phosphoric acid solution. The crushed sodium dihydrogen phosphate is not easy to agglomerate for subsequent reaction, inert gas is filled into the crushed sodium dihydrogen phosphate to prevent oxidation, the temperature of the crushed sodium dihydrogen phosphate is slowly reduced to room temperature after the sodium dihydrogen phosphate is calcined once to prevent agglomeration, and the crushed sodium dihydrogen phosphate is calcined again to accelerate the reaction and improve the purity of the sodium trimetaphosphate on the other hand.
Detailed Description
The present invention is further described below.
Example 1
Adding phosphoric acid solution into a reaction kettle, stirring, slowly adding sodium hydroxide, detecting the pH range to be 3.0 on line, heating to 40 ℃, and reacting for 3 hours. And (3) after the reaction is finished, crystallizing, cooling to 0 ℃ while stirring, adding the reaction solution into a centrifugal machine after stirring for 2 hours, throwing and filtering until no liquid flows out, adding 90% ethanol into the centrifugal machine, continuing throwing and filtering, collecting a filter cake after no liquid flows out, putting the filter cake into a blast oven, setting the temperature to be 60 ℃, and drying for 5 hours to obtain the anhydrous sodium dihydrogen phosphate. Crushing in a crusher to obtain anhydrous sodium dihydrogen phosphate granule with purity of 98.5%. And adding anhydrous sodium dihydrogen phosphate particles into the crucible, filling nitrogen, heating to 200 ℃, calcining for 4 hours, and finishing the reaction. Slowly cooling to room temperature, and pulverizing into granules with a pulverizer. The crucible is placed again, nitrogen gas is filled in the crucible, the crucible is heated to 560 ℃, and the calcination is continued for 7 hours. And cooling to room temperature to obtain sodium trimetaphosphate solid. Pulverizing the solid sodium trimetaphosphate with a pulverizer, and sieving with a sieve to obtain particles of 5-10 μm to obtain sodium trimetaphosphate as toothpaste abradant.
Example 2
Adding phosphoric acid solution into a reaction kettle, stirring, slowly adding sodium hydroxide, detecting the pH range to be 4.5 on line, heating to 60 ℃, and reacting for 2 hours. And after the reaction is finished, crystallizing, cooling to 10 ℃ while stirring, stirring for 3 hours, adding the reaction liquid into a centrifugal machine, throwing and filtering until no liquid flows out, adding 95% ethanol into the centrifugal machine, continuing throwing and filtering, collecting a filter cake after no liquid flows out, putting the filter cake into a blast oven, setting the temperature to be 70 ℃, and drying for 4 hours to obtain the anhydrous sodium dihydrogen phosphate. Placing the mixture into a crusher to be crushed to obtain anhydrous sodium dihydrogen phosphate particles with the purity of 99.0 percent. Adding anhydrous sodium dihydrogen phosphate particles into a crucible, filling helium, heating to 240 ℃, calcining for 3 hours, and finishing the reaction. Slowly cooling to room temperature, and pulverizing into granules with a pulverizer. And putting the mixture into the crucible again, filling inert gas, heating the mixture to 600 ℃, and continuing calcining the mixture for 5 hours. And cooling to room temperature to obtain sodium trimetaphosphate solid. Pulverizing the solid sodium trimetaphosphate with a pulverizer, and sieving with a sieve to obtain particles of 5-10 μm to obtain sodium trimetaphosphate as toothpaste abradant.
Example 3
Adding phosphoric acid solution into a reaction kettle, stirring, slowly adding sodium carbonate, detecting the pH range to be 4.5 on line, heating to 45 ℃, and reacting for 2.5 hours. And after the reaction is finished, crystallizing, cooling to 5 ℃ while stirring, stirring for 2.5 hours, adding the reaction liquid into a centrifugal machine, throwing and filtering until no liquid flows out, adding 95% ethanol into the centrifugal machine, continuing to throw and filter, collecting filter cakes after no liquid flows out, putting the filter cakes into a blast oven, setting the temperature to be 65 ℃, and drying for 4.5 hours to obtain the anhydrous sodium dihydrogen phosphate. Placing the mixture into a crusher to be crushed to obtain anhydrous sodium dihydrogen phosphate particles with the purity of 99.8 percent. Adding anhydrous sodium dihydrogen phosphate particles into a crucible, introducing nitrogen, heating to 220 ℃, calcining for 3.5 hours, and finishing the reaction. Slowly cooling to room temperature, and pulverizing into granules with a pulverizer. And putting the mixture into the crucible again, filling inert gas, heating the mixture to 580 ℃, and continuing calcining the mixture for 6 hours. And cooling to room temperature to obtain sodium trimetaphosphate solid. Pulverizing the solid sodium trimetaphosphate with a pulverizer, and sieving with a sieve to obtain particles of 5-10 μm to obtain sodium trimetaphosphate as toothpaste abradant.
Example 4
Adding phosphoric acid solution into a reaction kettle, stirring, slowly adding sodium bicarbonate, detecting the pH range to be 4.0 on line, heating to 60 ℃, and reacting for 2 hours. And after the reaction is finished, crystallizing, cooling to 10 ℃ while stirring, stirring for 3 hours, adding the reaction liquid into a centrifugal machine, throwing and filtering until no liquid flows out, adding 95% ethanol into the centrifugal machine, continuing throwing and filtering, collecting a filter cake after no liquid flows out, putting the filter cake into a blast oven, setting the temperature to be 70 ℃, and drying for 4 hours to obtain the anhydrous sodium dihydrogen phosphate. Placing the mixture into a crusher to be crushed to obtain anhydrous sodium dihydrogen phosphate particles with the purity of 99.0 percent. Adding anhydrous sodium dihydrogen phosphate particles into a crucible, introducing nitrogen, heating to 200 ℃, calcining for 4 hours, and finishing the reaction. Slowly cooling to room temperature, and pulverizing into granules with a pulverizer. And putting the mixture into the crucible again, filling inert gas, heating the mixture to 560 ℃, and continuing calcining the mixture for 7 hours. And cooling to room temperature to obtain sodium trimetaphosphate solid. And (3) crushing the sodium trimetaphosphate solid by using a crusher, and screening 5-10 micron particles by using a screen to obtain the sodium trimetaphosphate as the toothpaste abradant.

Claims (9)

1. A production method of sodium trimetaphosphate used as an abrasive agent for toothpaste is characterized by comprising the following steps: adding phosphoric acid solution into a reaction kettle, stirring, slowly adding sodium salt, detecting the pH range to be 3.0-4.5 on line, heating to 40-60 ℃, and reacting for 2-3 hours. And after the reaction is finished, crystallizing, cooling to 0-10 ℃ while stirring, stirring for 2-3 hours, adding the reaction liquid into a centrifugal machine, throwing and filtering until no liquid flows out, adding ethanol into the centrifugal machine to wash excessive phosphoric acid, continuing throwing and filtering, collecting filter cakes after no liquid flows out, putting the filter cakes into an oven, setting the temperature to be 60-70 ℃, and drying for 4-5 hours to obtain the anhydrous sodium dihydrogen phosphate. Pulverizing in pulverizer to obtain anhydrous sodium dihydrogen phosphate granule with purity of 98.5-99.8%. Step two: adding anhydrous sodium dihydrogen phosphate particles into a crucible, filling inert gas, heating to the temperature of 200-240 ℃, calcining for 3-4 hours, and finishing the reaction. Slowly cooling to room temperature, and pulverizing into granules with a pulverizer. And putting the mixture into the crucible again, filling inert gas, heating the mixture to the temperature of 560 ℃ and 600 ℃, and continuing calcining the mixture for 5 to 7 hours. And cooling to room temperature to obtain sodium trimetaphosphate solid. Step three: and (3) crushing the solid sodium trimetaphosphate by using a crusher, and screening particles by using a screen to obtain the sodium trimetaphosphate as the abrasive for the toothpaste.
2. The method for producing sodium trimetaphosphate as abrasive agent for toothpaste according to claim, wherein the sodium salt used in the first step is sodium hydroxide, sodium bicarbonate or sodium carbonate.
3. The method for producing sodium trimetaphosphate for toothpaste as an abrasive according to claim, wherein the centrifuge used in the first step is a preservative centrifuge.
4. The method for producing sodium trimetaphosphate as abrasive agent for toothpaste according to claim, wherein the ethanol concentration used in the first step is 90-95%.
5. The method for producing sodium trimetaphosphate for toothpaste as an abrasive according to claim, wherein the first oven is a forced air oven.
6. The method for producing sodium trimetaphosphate for toothpaste as an abrasive according to claim, wherein the crucible used in the second step is closed.
7. The method for producing sodium trimetaphosphate as abrasive agent for toothpaste according to claim, wherein the inert gas used in the second step is nitrogen or helium.
8. The method for producing sodium trimetaphosphate as abrasive agent for toothpaste according to claim, wherein the pulverizer used in the second step is a jet mill.
9. The method for producing sodium trimetaphosphate as abrasive agent for toothpaste according to claim, wherein the diameter of the brush used in step two is 5-10 μm.
CN202110494256.2A 2021-05-07 2021-05-07 Production method of sodium trimetaphosphate as abrasive for toothpaste Pending CN113133949A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115159488A (en) * 2022-07-22 2022-10-11 承德莹科精细化工股份有限公司 Preparation method of high-water-solubility glass-state sodium metaphosphate
CN117069083A (en) * 2023-09-21 2023-11-17 江苏恒世食品科技有限公司 Method for producing sodium trimetaphosphate by returning charge polymerization

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张越等: "三偏磷酸钠的制备及其作为磷酸化试剂的应用", 《无机盐工业》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115159488A (en) * 2022-07-22 2022-10-11 承德莹科精细化工股份有限公司 Preparation method of high-water-solubility glass-state sodium metaphosphate
CN115159488B (en) * 2022-07-22 2023-06-30 承德莹科精细化工股份有限公司 Preparation method of high water-solubility glassy sodium metaphosphate
CN117069083A (en) * 2023-09-21 2023-11-17 江苏恒世食品科技有限公司 Method for producing sodium trimetaphosphate by returning charge polymerization

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Application publication date: 20210720