CN100360418C - Process for producing toothpaste grade light-weight calcium carbonate - Google Patents
Process for producing toothpaste grade light-weight calcium carbonate Download PDFInfo
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- CN100360418C CN100360418C CNB2005100500817A CN200510050081A CN100360418C CN 100360418 C CN100360418 C CN 100360418C CN B2005100500817 A CNB2005100500817 A CN B2005100500817A CN 200510050081 A CN200510050081 A CN 200510050081A CN 100360418 C CN100360418 C CN 100360418C
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Abstract
The present invention relates to a method for producing toothpaste grade light calcium carbonate. The method mainly comprises the following steps of hydrating lime CaO by warm water to generate Ca(OH)2 serous fluid, enabling the Ca(OH)2 serous fluid to pass through a sieve with small mesh number and a sieve with a large mesh number for at least more than two times and pass through a hydraulic cyclone, enabling the baume degree of raw slurry to reach 10 to 14 Be degrees, delivering the Ca(OH)2 serous fluid into a carbonization tower, carrying out reactions by leading in the mixed gas of CO2 and N2, adding crystal shape control agents and desulfurizing agents at a solution temperature of 50 DEG C, leading in kiln gas with a CO2 concentration of 14 to 20%, orderly adding desulfurizing agents, metallic ion chelators, disinfectants and pH regulating agents after reactions, keeping the mixtures for 4 hours, centrifugally dewatering and drying the mixtures to obtain calcium carbonate. The present invention has the advantages of high yield, high product whiteness and few harmful substances, such as heavy metal, etc., and the quality indexes come up to the leading level of foreign products. The slurry feeding time is automatically controlled by adding reagents to ensure the complete crystal shape and the uniform crystal size of the generated calcium carbonate.
Description
Technical field
The present invention relates to a kind of chemical synthesis process, especially a kind of is the production method of the toothpaste grade light-weight calcium carbonate of raw material with calcium hydroxide.
Background technology
Light calcium carbonate is a kind of inorganic chemical product with extensive use, traditional and common toothpaste is all using as raw material with water-ground limestone, and clinic study shows, the toothpaste that water-ground limestone is produced is very big to the glaze surface wear of tooth, and harmful substance contents such as heavy metal are very high, do not play good dental care benefits.In recent years, the higher producer (as U.S. Colgare company etc.) of popularity with water-ground limestone gradate for light calcium carbonate be raw material.Traditional Production of Light Calcium Carbonate counterweight metal index is difficult to control, and objectionable impuritiess such as impurity and heavy metal are more.
Summary of the invention
Purpose of the present invention will solve above-mentioned described deficiency exactly, and a kind of production method of toothpaste grade light-weight calcium carbonate is provided.Chemical property good stability, the purity height of the light calcium carbonate of producing, objectionable constituent such as impurity and heavy metal are few, and complete crystalline structure (being spindle shape or spherical) is arranged, even particle size distribution, the light calcium carbonate of suitable toothpaste production usefulness.
The present invention solves the technical scheme that its technical problem adopts.The production method of this toothpaste grade light-weight calcium carbonate mainly may further comprise the steps: 1), water 5-10 by volume under 10 ℃-50 ℃ excessively with filter process: 1 generates Ca (OH) with lime CaO after hydration reaction
2Slurries, described lime are calcined down at 1000-1100 ℃ by Wingdale and are obtained; 2), Ca (OH)
2Slurries to the big screen cloth of the above different meshes of secondary at least that passes through, are removed Ca (OH) according to little
2Impurity in the slurries obtains epigranular, the highly purified slurry of giving birth to, and by wet cyclone, further removes impurity, comprises nonmetal silicon, heavy metals such as lead, and the degree Beaume of giving birth to slurry reaches 10-14Be; 3), Ca (OH)
2Slurries are squeezed into carbonating tower by volume pump, feed CO from the carbonating tower bottom
2, N
2Gas mixture reacts, and when treating that solution temperature rises to 50 ℃, adds crystal control agent and desulfuration agent, feeds CO in solution
2, be 7 until the pH value, after reaction finishes, added desulfuration agent, metal ion chelation agent, sterilizing agent, pH value conditioning agent successively 4 hours afterwards, product is filtered carry out centrifuge dehydration, at 100-120 ℃ of temperature drying, obtain lime carbonate; This is reflected at liquid phase and carries out, and adopts the continous way process, and its concrete operations condition is carbonization pressure: 0.07-0.09MPa, CO in the kiln gas
2Concentration is 14-20%, carbonization temperature 50-60 ℃.
Described crystal control agent is brown sugar or glucose, and the volume percent of add-on is 0.35%; The desulfuration agent is a hydrogen peroxide, and the volume percent of add-on is 0.3% for the first time, and the volume percent of add-on is 0.07% for the second time; The metal ion chelating is a Sodium hexametaphosphate 99, and the volume percent of add-on is 0.004%; Sterilizing agent is a chlorinated lime, and the volume percent of add-on is 0.09%; PH value conditioning agent is a phosphoric acid, and the volume percent of add-on is 0.3%.
Effect of the present invention is: replace common coal pit with the combustion gas shaft kiln, replaced traditional coal fuel sintering technology with liquefied gas, use this technology, heavy metal in the coal and other detrimental impurity can not brought in the product, and reasonably control calcining temperature 1000-1100 ℃, automatically control the into slurry time by the reagent that adds, crystal shape complete (being spindle shape or spherical), the crystallographic dimension of guaranteeing to generate lime carbonate are even.By the output capacity of method finished product of the present invention higher (be traditional fine particle calcium carbonate 1.1 times), the product whiteness height, objectionable impuritiess such as heavy metal are atomic, and its quality index reaches the top standard of external product.Use liquefied gas to be fuel, selectivity is good, and by product is few, and the output of waste gas is atomic or do not have the three wastes that produce in this products production, treated allow compliance with emission standards.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment 1: the production method of this toothpaste grade light-weight calcium carbonate mainly may further comprise the steps:
1), the water of crossing with filter process generated Ca (OH) with lime CaO in 7: 1 by volume after hydration reaction under 40 ℃
2Slurries, described lime are calcined down at 1000-1100 ℃ by Wingdale and are obtained; Wherein Wingdale employing high purity, heavy metal and the atomic fine and close Wingdale of impurity amount thereof are raw material, and specific targets are as follows: purity 〉=99.5%, heavy metal≤20ppm, iron level≤80ppm, lead content≤2ppm, arsenic content≤2ppm, Mg content≤0.3%.
2), Ca (OH)
2Slurries are respectively 125 orders, 200 orders and 320 orders according to the little screen cloth that arrives big by three different meshes, remove Ca (OH)
2Impurity in the slurries obtains epigranular, the highly purified slurry of giving birth to, and by wet cyclone, further removes impurity, comprises nonmetal silicon, and heavy metals such as lead, degree Beaume reach 11.5Be ° of Ca (OH)
21500 milliliters of solution;
3), Ca (OH)
2Slurries are squeezed into carbonating tower by volume pump, feed CO from the carbonating tower bottom
2, N
2Gas mixture reacts, and when treating that solution temperature rises to 50 ℃, adds crystal control agent brown sugar 0.35% (volume percent) and desulfuration agent hydrogen peroxide 0.3% (volume percent), feeds CO in solution
2Until the pH value is 7, after reaction finishes, adding volume percent successively is desulfuration agent hydrogen peroxide 0.07%, after the metal ion chelating Sodium hexametaphosphate 99 0.004%, sterilizing agent chlorinated lime 0.09%, pH value conditioning agent phosphoric acid 0.3% 4 hours, centrifuge dehydration is carried out in the product filtration,, obtained 258g lime carbonate at 120 ℃ of temperature dryings; Use the sem observation crystal formation, median size is the spindle-type light calcium carbonate of 5.5 μ m, meets the toothpaste production requirement.
This is reflected at liquid phase and carries out, and adopts the continous way process, and its concrete operations condition is carbonization pressure: 0.07-0.09MPa, CO in the kiln gas
2Concentration is 14-20%, carbonization temperature 50-60 ℃.After the dehydration workshop section in step 3), form strict microorganism supervisory system, prevent the pollution of artificial or implements etc. by sterilization equipments such as ultraviolet ray or infrared lights, total plate count is controlled at≤100fu/g in the microbiological indicator the most at last, must not find the blue formula negative bacillus of mould, yeast and leather in detection.
Embodiment 2:
Crystal control agent brown sugar among the embodiment 1 is replaced with glucose, and other conditions are all identical with example 1, obtain lime carbonate 255g, and the crystal median size is the spindle-type light calcium carbonate of 5.2 μ m, meets the toothpaste production requirement.
Embodiment 3:
Be with the difference of embodiment 1: the warm water with the CaO that generates in the kiln and 35 ℃ is made into the Ca that degree Beaume is 11.5Be (OH)
28 tons of solution, treat to add when solution temperature is 50 ℃ brown sugar 0.35% (volume percent, down together), hydrogen peroxide 0.3% is sent in the carbonating tower again, and feeding gas concentration lwevel at the bottom of tower is the kiln gas of 14-20%, pressure is 0.07-0.09MPa, until the pH value is 7, and temperature is about 60 ℃, lasts 1 hour, after reaction finishes, add hydrogen peroxide 0.07% successively, Sodium hexametaphosphate 99 0.004%, chlorinated lime 0.09%, phosphoric acid 0.3% 4 hours afterwards, centrifuge dehydration then at 120 ℃ of temperature dryings, obtains toothpaste grade light-weight calcium carbonate.Use the sem observation crystalline form, median size is the spindle-type light calcium carbonate of 5.5 μ m, and following the tracks of check point in process of production has: ore, water, CaO, CO
2, Ca (OH)
213 of slurries, carbonization slurries, pulp storage tank (giving birth to slurry, ripe slurry), dehydration powder, oven dry powder, work in-process, finished products etc.After the dehydration workshop section, form strict microorganism supervisory system, prevent the pollution of artificial or implements etc. by sterilization equipments such as ultraviolet ray, infrared lights, the total plate count in the microbiological indicator is controlled at≤100fu/g the most at last, and mould, yeast, the blue formula negative bacillus of leather must not be found in detection.
The contrast of table 1 lime carbonate physical and chemical index
| Sequence number | Project | Index | Example one | Example two | Example three |
| 1 | Lime carbonate is (with CaCO 3Meter) (in butt), % 〉= | 98.5 | 98.7 | 98.6 | 98.6 |
| 2 | Volatile content below 105 ℃, %≤ | 0.5 | 0.2 | 0.2 | 0.1 |
| 3 | PH value (20% turbid liquid) | 8.5-9.5 | 9.3 | 9.4 | 9.0 |
| 4 | Hydrochloric acid acid non-soluble substance content, % | 0.2 | 0.1 | 0.1 | 0.1 |
| 5 | Free alkali content (in Na2O), % | 0.07 | 0.07 | 0.07 | 0.07 |
| 6 | Fe content, % | 0.01 | 0.01 | 0.01 | 0.01 |
| 7 | Magnesium (Mg) content, % | 0.3 | 0.15 | 0.2 | 0.1 |
| 8 | Whiteness, degree | 94 | 94.5 | 94.7 | 95 |
| 9 | Settling volume, ml/g | 1.7-2.1 | 1.9 | 2.0 | 1.8 |
| 10 | Sieve thing (crossing the 45um testing sieve), % | 99.9 | 100.0 | 100.0 | 100.0 |
| 11 | Heavy metal (in Pb) content, % | 0.002 | ＜0.002 | ＜0.002 | ＜0.002 |
| 12 | Barium (Ba) content | By | By | By | By |
| 13 | Chloride content, % | 0.005 | ＜0.005 | ＜0.005 | ＜0.005 |
| 14 | Apparent density, g/ml | 0.64-0.75 | 0.7 | 0.72 | 0.68 |
| 15 | Sulfide | Must not detect | Do not detect | Do not detect | Do not detect |
The contrast of table 2 lime carbonate sanitary index
| Sequence number | Project | Index | Example one | Example two | Example three |
| 1 | Plumbous (Pb) content, %≤ | 0.0002 | 0.0001 | 0.0001 | 0.0001 |
| 2 | Arsenic (As) content, %≤ | 0.0002 | ＜0.0001 | ＜0.0001 | ＜0.0001 |
| 3 | Total plate count, cfu/g≤ | 100 | 50 | 65 | ＜10 |
| 4 | Mould and yeast, cfu/g≤ | 100 | 60 | 70 | ＜10 |
| 5 | Streptococcus aureus | Must not detect | Do not detect | Do not detect | Do not detect |
| 6 | Remove from office blue formula negative bacillus | Must not detect | Do not detect | Do not detect | Do not detect |
Claims (7)
1, a kind of production method of toothpaste grade light-weight calcium carbonate is characterized in that: mainly may further comprise the steps:
1), the water of crossing with filter process 5-10 by volume under 10 ℃-50 ℃: 1 generates Ca (OH) with lime after hydration reaction
2Slurries, described lime are calcined down at 1000-1100 ℃ by Wingdale and are obtained;
2), Ca (OH)
2Slurries to the big screen cloth of the above different meshes of secondary at least that passes through, are removed Ca (OH) according to little
2Impurity in the slurries obtains epigranular, the highly purified slurry of giving birth to, and by wet cyclone, further removes impurity, and the degree Beaume of giving birth to slurry reaches 10-14Be °;
3), Ca (OH)
2Slurries are squeezed into carbonating tower by volume pump, feed CO from the carbonating tower bottom
2, N
2Gas mixture reacts, and when treating that solution temperature rises to 50 ℃, adds crystal control agent and desulfuration agent, feeds CO in solution
2, be 7 until the pH value, after reaction finishes, added desulfuration agent, metal ion chelation agent, sterilizing agent, pH value conditioning agent successively 4 hours afterwards, product is filtered carry out centrifuge dehydration, at 100-120 ℃ of temperature drying, obtain lime carbonate; This is reflected at liquid phase and carries out, and adopts the continous way process, and its concrete operations condition is carbonization pressure: 0.07-0.09MPa, CO in the kiln gas
2Concentration is 14-20%, carbonization temperature 50-60 ℃.
2, the production method of toothpaste grade light-weight calcium carbonate according to claim 1 is characterized in that: it is raw material that described Wingdale adopts the fine and close Wingdale of purity 〉=99.5%, heavy metal≤20ppm.
3, the production method of toothpaste grade light-weight calcium carbonate according to claim 1 is characterized in that: in step 2) described in Ca (OH)
2Slurries to big screen cloth by three different meshes, are respectively 125 orders, 200 orders and 320 orders according to little.
4, the production method of toothpaste grade light-weight calcium carbonate according to claim 1, it is characterized in that: after the dehydration workshop section in step 3), by ultraviolet ray or the disinfection of infrared light sterilization equipment, total plate count is controlled at≤100fu/g in the microbiological indicator the most at last, must not find the blue formula negative bacillus of mould, yeast and leather in detection.
5, the production method of toothpaste grade light-weight calcium carbonate according to claim 1 is characterized in that: described product shape control agent is brown sugar or glucose.
6, the production method of toothpaste grade light-weight calcium carbonate according to claim 1 is characterized in that: described desulfuration agent, metal ion chelation agent, sterilizing agent, pH value conditioning agent are respectively hydrogen peroxide, Sodium hexametaphosphate 99, chlorinated lime and phosphoric acid.
7, according to the production method of claim 1 or 6 described toothpaste grade light-weight calcium carbonates, it is characterized in that: described crystal control agent is brown sugar or glucose, and the volume percent of add-on is 0.35%; The desulfuration agent is a hydrogen peroxide, and the volume percent of add-on is 0.3% for the first time, and the volume percent of add-on is 0.07% for the second time; The metal ion chelating is a Sodium hexametaphosphate 99, and the volume percent of add-on is 0.004%; Sterilizing agent is a chlorinated lime, and the volume percent of add-on is 0.09%; PH value conditioning agent is a phosphoric acid, and the volume percent of add-on is 0.3%.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101838674A (en) * | 2009-03-19 | 2010-09-22 | 上海融氏企业有限公司 | Production method of starch sugar |
| CN102432054A (en) * | 2011-09-28 | 2012-05-02 | 建德市云峰碳酸钙有限公司 | Method for producing light calcium carbonate slurry and light calcium carbonate paste |
| CN104477961A (en) * | 2014-12-22 | 2015-04-01 | 南通市飞宇精细化学品有限公司 | Preparation method of high-purity fine calcium carbonate |
| CN105016369A (en) * | 2014-12-30 | 2015-11-04 | 建德市云峰碳酸钙有限公司 | Production method for pasty calcium carbonate for papermaking |
| CN106365190B (en) * | 2016-08-26 | 2019-01-11 | 石家庄市东升钙业有限公司 | The preparation method of medicine fermentation calcium carbonate |
| CN107459053A (en) * | 2017-08-10 | 2017-12-12 | 青阳县永诚钙业有限责任公司 | A kind of production method of paste calcium carbonate |
| CN114620753B (en) * | 2021-11-29 | 2023-08-18 | 浙江天石纳米科技股份有限公司 | Low-carbon process method for producing light calcium carbonate by comprehensively utilizing chemical reaction heat |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1193602A (en) * | 1997-03-17 | 1998-09-23 | 北京化工大学 | Preparation of lightweight calcium carbonate |
| CN1417126A (en) * | 2002-12-13 | 2003-05-14 | 黄木清 | Non-cooling process of producing nano calcium carbonate |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1193602A (en) * | 1997-03-17 | 1998-09-23 | 北京化工大学 | Preparation of lightweight calcium carbonate |
| CN1417126A (en) * | 2002-12-13 | 2003-05-14 | 黄木清 | Non-cooling process of producing nano calcium carbonate |
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Owner name: ZHEJIANG TIANSHI NANOTECHNOLOGY CO., LTD. Free format text: FORMER OWNER: TIANSHI CALCIUM CARBONATE CO., LTD., JIANDE CITY Effective date: 20140423 |
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Free format text: CORRECT: ADDRESS; FROM: 311607 HANGZHOU, ZHEJIANG PROVINCE TO: 311600 HANGZHOU, ZHEJIANG PROVINCE |
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Effective date of registration: 20140423 Address after: 311600, Zhejiang Province, Jiande City, lower Town, lower village, Creek Village on the stream Patentee after: TIANSHI CALCIUM CARBONATE CO., LTD. Address before: 311607 Xin'An River Street, east of Xin'An River town, Zhejiang City, Jiande Province Patentee before: Jiande Tianshi Calcium Carbonate Co., Ltd. |
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Address after: 311600 Xiawa village, Xiawa Town, Jiande City, Zhejiang Province Patentee after: ZHEJIANG TIANSHI NANO-TECH Co.,Ltd. Address before: 311600 Xiawa village, Xiawa Town, Jiande City, Zhejiang Province Patentee before: TIANSHI CALCIUM CARBONATE Co.,Ltd. |