CN1301904C - Process for preparing silicon dioxide for green high transparent toothpaste - Google Patents
Process for preparing silicon dioxide for green high transparent toothpaste Download PDFInfo
- Publication number
- CN1301904C CN1301904C CNB2005100124804A CN200510012480A CN1301904C CN 1301904 C CN1301904 C CN 1301904C CN B2005100124804 A CNB2005100124804 A CN B2005100124804A CN 200510012480 A CN200510012480 A CN 200510012480A CN 1301904 C CN1301904 C CN 1301904C
- Authority
- CN
- China
- Prior art keywords
- preparing
- phosphoric acid
- toothpaste
- aluminum sulfate
- acidifying agent
- 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.)
- Expired - Fee Related
Links
Abstract
The present invention relates to silicon dioxide for green high transparent toothpaste, which is prepared by an acidifying agent and an alkaline silicate solution. In raw materials, food-grade aluminium sulfate and phosphoric acid are adopted as addition agents to obviously enhance the light transmittance of the prepared precipitated silicon dioxide. All through the processes of the preparation, deionized water is adopted to prepare products with few impurities and high purity. The control of technological parameter is strict so as to prepare products with high stability and good flow performance. When the temperature of operating environment is changed, the toothpaste can not harden or soften, thereby satisfying the technological requirement of high-grade transparent toothpaste. The various parameters of the prepared toothpaste are all conform to or superior to the trade standard. The silicon dioxide for green high transparent toothpaste has a significance for satisfying the requirements of domestic high-grade toothpaste preparation and substitutes for imported goods.
Description
Technical Field
The invention belongs to superfine silicon dioxide for toothpaste production, and particularly relates to a preparation method for producing green high-transparency silicon dioxide for toothpaste by adopting a precipitation method.
Background
In order to adapt to the development direction of multifunctional and high added value of toothpaste products, toothpaste technology is also continuously innovated. Transparent toothpaste is made of novel soft abrasive, which is silicon dioxide produced by precipitation method, and has been rapidly popularized and applied in China due to its good performance. The production of transparent toothpaste requires high light transmittance, low refractive index and strict requirements for process and raw materials of the precipitated silica. At present, the light transmittance of the domestic precipitated silica is about 70 percent, the domestic precipitated silica can not meet the market demand of high-grade transparent toothpaste, and most of the domestic precipitated silica for the high-grade transparent toothpaste depends on import.
The preparation of precipitated silica is divided into a gas phase method and a precipitation method. The gas phase method has the advantages of high price, less dosage, relatively low cost of the precipitation method and wide application range.
In the prior art, the production of silica by precipitation method usually comprises adding concentrated sulfuric acid and sodium silicate in a reaction kettle according to a weight ratio for reaction, cooling the reacted materials, pumping the materials into a filter press by a pump for filtering, washing and drying to make liquid-solid two phases reach a certain ratio, pulping the filter cake under high pressure, curing, storing in a concentrated slurry tank, and drying to obtain silica.
The precipitated silica produced by the method has poor stability and is easy to cause the toothpaste to become hard; low transparency and purity, and is not suitable for the production of high-grade transparent toothpaste.
The toothpaste-grade silicon dioxide is a novel functional material grown after the traditional inorganic material is upgraded by the industry and the product structure is adjusted in the chemical industry. The obvious advantages of toothpaste grade silicon dioxide in the field of daily chemicals such as toothpaste, cosmetics and the like and the irreplaceability of the chemical structure and the performance of the toothpaste grade silicon dioxide become the hot field of international scientific research and technical development at present. With the development of fine chemical ultrafine functional materials in China, the development of toothpaste grade silicon dioxide with independent intellectual property rights becomes one of the key research subjects of numerous scientific researchers.
Through domestic online search, no patent literature report of precipitated silica for toothpaste, which is the same as the production method of the invention, is found at present.
Disclosure of Invention
The invention mainly solves the technical problem that the additive is adopted to further improve the purity of the raw materials, so that the produced precipitated silica meets the raw material requirement of the high-transparency toothpaste; by optimizing and controlling the technological parameters, the green high-transparency toothpaste silicon dioxide which is highly dispersed, pure, fine and amorphous and has good stability is obtained.
The main raw materials of the silicon dioxide for preparing the green high-transparency toothpaste are sodium silicate and sulfuric acid, and the reaction equation is as follows:
the preparation method of the silicon dioxide for the green high-transparency toothpaste comprises the following steps:
A. preparing an acidifier: adding 1.08ml/g aluminum sulfate into 3.0-4.5N sulfuric acid, wherein the volume ratio of concentrated sulfuric acid to aluminum sulfate is 1-4: 1.
B. Preparing an alkali silicate solution: sodium silicate with the concentration of 1.2-2.2N and phosphoric acid with the concentration of 10%, wherein 0.05-0.1 cubic of phosphoric acid is added into each cubic of sodium silicate.
C. Adding 3000-4000L of the alkali silicate solution into a reaction kettle, stirring, uniformly heating to 80-90 ℃, adding an acidifying agent, controlling the flow rate of the acidifying agent to be 2-3 m3/h, reacting for 25-45 min, and aging for 20min when the pH value reaches 7.5-9; and (3) continuously adding an acidifying agent, controlling the flow rate to be 1-1.5 m3/h, acidifying for 5-8 min, continuously stirring for 10min when the pH value reaches 4-5, then pumping the slurry into a curing tank, curing for 30min, filtering, washing, drying and crushing to obtain a final product, namely 1000-mesh white powder, namely precipitated silicon dioxide.
Deionized water is adopted as the process water for preparing the raw materials.
The aluminum sulfate and the phosphoric acid in the raw materials belong to food additives.
In the invention, food-grade aluminum sulfate and phosphoric acid are used as additives in raw materials, so that the light transmittance of the produced precipitated silicon dioxide is obviously improved; deionized water is adopted in the preparation process, so that the produced product has less impurities and high purity; the technological parameters are strictly controlled, so that the product has high stability and good fluidity, and the produced toothpaste body does not become hard and soft when the temperature of the use environment changes, and can meet the technological requirements of high-grade transparent toothpaste.
The green high-transparency silica for toothpaste produced by the invention has the characteristics of controllable structure, low specific surface area, high filling density and the like. All technical performance indexes can meet the process requirements of high-grade transparent toothpaste, wherein the content of silicon dioxide is more than or equal to 96 percent, heavy metal (calculated by pb) is less than or equal to 20ppm, heating decrement is less than or equal to 8.0 percent, ignition decrement is less than or equal to 8.0 percent, pH is 6.5-8.5, refractive index is 1.440-1.465N, light transmittance is more than or equal to 95 percent, water absorption is 17-34ml/20g, and granularity: 200 meshes of undersize products are more than or equal to 99.5 percent, 320 meshes are more than or equal to 98 percent, the total number of bacteria is less than 100cfu/g, and the above parameters meet or are superior to the industrial standard.
The invention adopts a unique process technology to produce the nontoxic, harmless and highly transparent precipitated silica for the toothpaste, and has important significance for meeting the production requirements of domestic high-grade toothpaste and replacing imported products.
Detailed Description
According to the preparation method of the green high-transparency silica for toothpaste, the invention can produce three types of transparent combination type, transparent friction type and transparent thickening type.
Example 1
The preparation method of the transparent combined precipitated silica comprises the following steps:
A. preparing an acidifier: adding 1.08ml/g aluminum sulfate into 3.9-4.2N sulfuric acid, wherein the volume ratio of concentrated sulfuric acid to aluminum sulfate is 4: 1.
B. Preparing an alkali silicate solution: sodium silicate with the concentration of 1.65-1.70N and phosphoric acid with the concentration of 10%, wherein 0.05-0.1 cubic of phosphoric acid is added into each cubic of sodium silicate.
C. Adding 3500L of the above alkaline silicate solution into a reaction kettle, stirring, uniformly heating to 86 + -1 deg.C, adding acidifying agent, and controlling the flow rateof acidifying agent at 3m3H, aging for 20min when the reaction time is 30-35 min and the pH value reaches 8-9; the acidifying agent was continuously added, and the flow rate was controlled at 1.5m3And h, acidifying for 5-8 min, continuing stirring for 10min when the pH value reaches 4-5, then pumping the slurry into a curing tank, curing for 30min, filtering, washing, drying and crushing to obtain a final product which is 1000-mesh white powder, namely the transparent combined precipitated silica.
Example 2
The preparation method of the transparent thickening type precipitated silica comprises the following steps:
A. preparing an acidifier: adding 1.08ml/g aluminum sulfate into 3.0-3.2N sulfuric acid, wherein the volume ratio of concentrated sulfuric acid to aluminum sulfate is 1: 1.
B. Preparing an alkali silicate solution: sodium silicate with the concentration of 1.20-1.40N and phosphoric acid with the concentration of 10%, wherein 0.05-0.1 cubic of phosphoric acid is added into each cubic of sodium silicate.
C. Adding 3500L of the above alkaline silicate solution into a reaction kettle, stirring, uniformly heating to 81 + -1 deg.C, adding acidifying agent and acidThe flow rate of the reagent is controlled to be 2m3H, aging for 20min when the reaction time is 40-45 min and the pH value reaches 7.5-7.8; adding acidifying agent continuously, and controlling the flow rate at 1m3And h, acidifying for 6-8 min, continuing stirring for 10min when the pH value reaches 4-4.5, then pumping the slurry into a curing tank, curing for 30min, filtering, washing, drying and crushing to obtain a final product which is 1000-mesh white powder, namely transparent thickening precipitated silica.
Example 3
The technological parameters for preparing the transparent friction type precipitated silica are as follows:
A. preparing an acidifier: adding 1.08ml/g aluminum sulfate into 4.0-4.2N sulfuric acid, wherein the volume ratio of concentrated sulfuric acid to aluminum sulfate is 4: 1.
B. Preparing an alkali silicate solution: sodium silicate with the concentration of 2-2.05N and phosphoric acid with the concentration of 10 percent, wherein 0.05-0.1 cubic of phosphoric acid is added into each cubic of sodium silicate.
C. Firstly, 1350-1400L of sodium sulfate solution with the concentration of 4-8% is added into a reaction kettle, the mixture is stirred, the temperature of the mixture is uniformly raised to 89 +/-1 ℃, the pH value of the mixture is adjusted to 9-10 by using the alkaline silicate solution, and meanwhile, an acidifying agent and the alkaline silicate solution are added. Wherein the flow rate of the alkali silicate solution is 5.5-6.0 m3H, the flow rate of the acidifying agent is controlled at 3m2H, aging for 20min when the reaction time is 25-30 min and the pH value reaches 9.0; the acidifying agent was continuously added, and the flow rate was controlled at 1.5m2And h, acidifying for 5-8 min, continuing stirring for 10min when the pH value reaches 4.5-4.7, then pumping the slurry into a curing tank, curing for 30min, filtering, washing, drying and crushing to obtain a final product which is 1000-mesh white powder, namely transparent friction type precipitated silica.
Deionized water is adopted as process water required in the preparation of the raw materials in the above embodiments, and aluminum sulfate and phosphoric acid in the raw materials belong to food additives.
Claims (5)
1. A preparation method of greenhigh-transparency silica for toothpaste is characterized by comprising the following steps:
A. preparing an acidifier: adding 1.08ml/g aluminum sulfate into 3.0-4.5N sulfuric acid, wherein the volume ratio of concentrated sulfuric acid to aluminum sulfate is 1-4: 1;
B. preparing an alkali silicate solution: sodium silicate with the concentration of 1.2-2.2N and phosphoric acid with the concentration of 10%, wherein 0.05-0.1 cubic of phosphoric acid is added into each cubic of sodium silicate;
C. adding 3000-4000L of the alkali silicate solution into a reaction kettle, stirring, uniformly heating to 80-90 ℃, adding an acidifying agent, and controlling the flow rate of the acidifying agent to be 2-3 m3H, aging for 20min when the reaction time is 25-45 min and the pH value reaches 7.5-9; continuously adding an acidifying agent, and controlling the flow rate to be 1-1.5 m3Acidifying for 5-8 min, continuing stirring for 10min when the pH value reaches 4-5, then pumping the slurry into a curing tank, curing for 30min, filtering, washing, drying and crushing to obtain a final product which is 1000-mesh white powder, namely precipitated silicon dioxide;
the aluminum sulfate and the phosphoric acid in the raw materials belong to food additives.
2. The method for preparing silica for green high transparent toothpaste according to claim 1, characterized in that the method for preparing the transparent combination type precipitated silica is as follows:
A. preparing an acidifier: adding 1.08ml/g aluminum sulfate into 3.9-4.2N sulfuric acid, wherein the volume ratio of concentrated sulfuric acid to aluminum sulfate is 4: 1;
B. preparing an alkali silicate solution: sodium silicate with the concentration of 1.65-1.70N and phosphoric acid with the concentration of 10%, wherein 0.05-0.1 cubic of phosphoric acid is added into each cubic of sodium silicate;
C. adding 3500L of the above alkaline silicate solution into a reaction kettle, stirring, uniformly heating to 86 + -1 deg.C, adding acidifying agent, and controlling the flow rate of acidifying agent at 3m3H, aging for 20min when the reaction time is 30-35 min and the pH value reaches 8-9; the acidifying agent was continuously added, and the flow rate was controlled at 1.5m3Acidifying for 5-8 min, continuing stirring for 10min when the pH value reaches 4-5, then pumping the slurry into a curing tank,aging for 30min, filtering, washing, and dryingDrying and crushing to obtain white powder of 1000 meshes, namely transparent combined precipitated silica;
the aluminum sulfate and the phosphoric acid in the raw materials belong to food additives.
3. The method for preparing silica for green high transparent toothpaste according to claim 1, characterized in that the transparent thickening type precipitated silica is prepared as follows:
A. preparing an acidifier: adding 1.08ml/g aluminum sulfate into 3.0-3.2N sulfuric acid, wherein the volume ratio of concentrated sulfuric acid to aluminum sulfate is 1: 1;
B. preparing an alkali silicate solution: sodium silicate with the concentration of 1.20-1.40N and phosphoric acid with the concentration of 10%, wherein 0.05-0.1 cubic of phosphoric acid is added into each cubic of sodium silicate;
C. adding 3500L of the above alkaline silicate solution into a reaction kettle, stirring, uniformly heating to 81 + -1 deg.C, adding acidifying agent, and controlling the flow rate of acidifying agent at 2m3H, aging for 20min when the reaction time is 40-45 min and the pH value reaches 7.5-7.8; adding acidifying agent continuously, and controlling the flow rate at 1m3Acidifying for 6-8 min, continuing stirring for 10min when the pH value reaches 4-4.5, then pumping the slurry into a curing tank, curing for 30min, filtering, washing, drying and crushing to obtain a final product which is 1000-mesh white powder, namely transparent thickening precipitated silica;
the aluminum sulfate and the phosphoric acid in the raw materials belong to food additives.
4. The method for preparing silica for green high transparent toothpaste according to claim 1, wherein the process parameters for preparing transparent abrasive type precipitated silica are as follows:
A. preparing an acidifier: adding 1.08ml/g aluminum sulfate into 4.0-4.2N sulfuric acid, wherein the volume ratio of concentrated sulfuric acid to aluminum sulfate is 4: 1;
B. preparing an alkali silicate solution: sodium silicate with the concentration of 2-2.05N and phosphoric acid with the concentration of 10%, wherein 0.05-0.1 cubic of phosphoric acid is added into each cubic of sodium silicate;
C. firstly, 1350-1400L of sodium sulfate solution with the concentration of 4-8% is added into a reaction kettle, the mixture is stirred, the temperature of the mixture is uniformly raised to 89 +/-1 ℃, the pH value of the mixture is adjusted to 9-10 by using the alkaline silicate solution, and meanwhile, an acidifying agent and the alkaline silicate solution are added; wherein the flow rate of the alkali silicate solution is 5.5-6.0 m3H, the flow rate of the acidifying agent is controlled at 3m3H, aging for 20min when the reaction time is 25-30 min and the pH value reaches 9.0; the acidifying agent was continuously added, and the flow rate was controlled at 1.5m3Acidifying for 5-8 min, continuing stirring for 10min when the pH value reaches 4.5-4.7, then pumping the slurry into a curing tank, curing for 30min, filtering, washing, drying and crushing to obtain a final product which is 1000-mesh white powder, namely transparent friction type precipitated silica;
the aluminum sulfate and the phosphoric acid in the raw materials belong to food additives.
5. The method for preparing the silica for the green high-transparency toothpaste as claimed in claim 1, wherein the process water required for preparing the raw materials is deionized water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100124804A CN1301904C (en) | 2005-04-27 | 2005-04-27 | Process for preparing silicon dioxide for green high transparent toothpaste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100124804A CN1301904C (en) | 2005-04-27 | 2005-04-27 | Process for preparing silicon dioxide for green high transparent toothpaste |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1693193A CN1693193A (en) | 2005-11-09 |
| CN1301904C true CN1301904C (en) | 2007-02-28 |
Family
ID=35352340
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100124804A Expired - Fee Related CN1301904C (en) | 2005-04-27 | 2005-04-27 | Process for preparing silicon dioxide for green high transparent toothpaste |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1301904C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107792861B (en) * | 2017-11-06 | 2018-08-28 | 广州市飞雪材料科技有限公司 | A kind of low index of refraction high transparency friction type silica and its preparation method and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59163306A (en) * | 1983-03-08 | 1984-09-14 | Taki Chem Co Ltd | Silica as tooth paste base and its preparation |
| CN1070891A (en) * | 1991-10-02 | 1993-04-14 | 尤尼利弗公司 | Silicon-dioxide |
| EP0666832A1 (en) * | 1992-10-28 | 1995-08-16 | Crosfield Joseph & Sons | Silicas. |
| US20030003040A1 (en) * | 2001-03-15 | 2003-01-02 | De Gussa Ag | Silica and silicate by precipitation at constant alkali number, and its use |
-
2005
- 2005-04-27 CN CNB2005100124804A patent/CN1301904C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59163306A (en) * | 1983-03-08 | 1984-09-14 | Taki Chem Co Ltd | Silica as tooth paste base and its preparation |
| CN1070891A (en) * | 1991-10-02 | 1993-04-14 | 尤尼利弗公司 | Silicon-dioxide |
| CN1131536A (en) * | 1991-10-02 | 1996-09-25 | 尤尼利弗公司 | Transparent toothpaste composition containing amorphous silica |
| EP0666832A1 (en) * | 1992-10-28 | 1995-08-16 | Crosfield Joseph & Sons | Silicas. |
| US20030003040A1 (en) * | 2001-03-15 | 2003-01-02 | De Gussa Ag | Silica and silicate by precipitation at constant alkali number, and its use |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1693193A (en) | 2005-11-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109161971A (en) | A method of calcium sulfate crystal whiskers are prepared by titanium gypsum | |
| CN111559752A (en) | Production method of nano calcium carbonate for PE direct film blowing | |
| CN1699164A (en) | Process for producing white carbon black and sodium sulphite by sodium sulfate method | |
| CN111777089A (en) | Preparation method of high-purity vaterite type calcium carbonate microspheres | |
| CN101565512A (en) | Nanometer rare-earth calcium-zinc-magnesium-aluminum PVC composite stabilizer | |
| CN1301904C (en) | Process for preparing silicon dioxide for green high transparent toothpaste | |
| CN101774594A (en) | Method for preparing modified acicular wollastonite | |
| CN1418810A (en) | Silicon dioxide produced by high-structure, low surface sedimentation method, and prepn. method for producing same | |
| CN108502911B (en) | Barite purifying and whitening agent and purifying and whitening method thereof | |
| CN1124716A (en) | Synthesis of 4A zeolite with kaolinite and preparing process thereof | |
| CN110817892A (en) | Preparation method of superfine white carbon black for coating paint | |
| CN1125778C (en) | Preparation of nanometer metal oxide material | |
| CN1115774A (en) | Prepn of silica white with opal and diatomite | |
| CN1868886A (en) | Production method of cryolite | |
| CN112279288B (en) | Continuous preparation method of modified calcium sulfate | |
| CN107324350A (en) | A kind of method for preparing nanoprecipitation silica using low-grade diatomite | |
| CN1194044C (en) | Preparation of silica white from silicon sol | |
| CN1562758A (en) | Technique of carbonating method for synthesizing cryolite | |
| CN1915830A (en) | Method for purifying Al13 in high yield | |
| CN112441592A (en) | Controllable preparation method of high-purity wollastonite fiber | |
| CN1868887A (en) | Preparation method of cryolite | |
| CN1257767C (en) | Nanometer titanium dioxide catalyst for absorbing ultraviolet-visible light and its preparation method and application | |
| CN115571886B (en) | Preparation method of low-oil-absorption low-specific-surface-area silicon dioxide | |
| CN109183497A (en) | A kind of paper grade (stock) nano-TiO2The preparation method of/wollastonite compound | |
| CN1277747C (en) | Method for producing aluminum fluoride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20081212 Address after: Shanxi province Hequ County town of large mouth Mao style Patentee after: Shandong Tond Chemical Co., Ltd. Address before: Shanxi province Hequ County town of large mouth Mao style Patentee before: Zhang Yunsheng |
|
| ASS | Succession or assignment of patent right |
Owner name: SHANXI TONGDE CHEMICAL ENGINEERING CO., LTD. Free format text: FORMER OWNER: ZHANG YUNSHENG Effective date: 20081212 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070228 Termination date: 20150427 |
|
| EXPY | Termination of patent right or utility model |