CN107827137B - A kind of preparation method of the cubic winnofil of big partial size - Google Patents
A kind of preparation method of the cubic winnofil of big partial size Download PDFInfo
- Publication number
- CN107827137B CN107827137B CN201711261405.0A CN201711261405A CN107827137B CN 107827137 B CN107827137 B CN 107827137B CN 201711261405 A CN201711261405 A CN 201711261405A CN 107827137 B CN107827137 B CN 107827137B
- Authority
- CN
- China
- Prior art keywords
- calcium carbonate
- cubic
- winnofil
- big
- partial size
- 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.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses a kind of preparation methods of big cubic winnofil of partial size, when milk of lime refines, after being aged 36~48h, lime milk density is adjusted to 1.050~1.065, temperature is adjusted to 15~20 DEG C, limekiln kiln gas is passed through into carburizing reagent kettle, carbon dioxide volume content is 25~35% in the kiln gas of limekiln, when reaction system conductivity is down to 0.5ms/cm, stop carburizing reagent, the compound organic metal screener of calcium carbonate dry weight 0.3~1.0% is added, stir 20~40min, 1~4h is kept in 55~90 DEG C of temperature ranges, again it is passed through limekiln kiln gas, until reaction system reaches carbonization terminal, the surface treating agent of calcium carbonate dry weight 2.0~5.0% is added, 30~60min is stirred to complete Surface treatment；Present invention process curing is high-efficient, can obtain the cubic winnofil of big partial size within a short period of time, and product dispersibility is excellent, reunites few, and size tunable, and present invention process simple possible, production cost is low, has preferable economic benefit.
Description
Technical field
The present invention relates to winnofil preparation technical field more particularly to a kind of cubic winnofils of big partial size
Preparation method.
Background technique
Winnofil is a kind of white, nontoxic, functional stuffing for having no irritating odor, be widely used in plastics, rubber,
The industries such as coating, sealant, ink and papermaking.The winnofil of different-grain diameter and different-shape is played in different filling systems
Different effects.As paper surface gloss and smoothness can be improved in fusiform winnofil；Needle-shaped or crystal whisker-shaped precipitates carbon
Sour calcium has high anisotropy, is filled in the products such as rubber, paper, can significantly improve the mechanical performance and body for taking phase direction
The rheological behavior of system；Nodular precipitation calcium carbonate is then a kind of ideal toughening material, and the shock resistance of product of rubber and plastic can be improved；
Cubic nanometer calcium carbonate is since with preferable rheological property and strengthening and toughening performance, application field is the most extensive.
It is small, higher than table energy that cubic nanometer calcium carbonate has the characteristics that partial size, but in major applications occasion without body of laws
The existing distinctive Modification effect of its nanoparticle, to find out its cause, mainly nanometer calcium carbonate forms largely in application process
Micron-sized aggregate, aggregate is bigger, easier to form stress concentration in material internal, to cause the fracture and mistake of material
Effect.
In addition, cubic nanometer calcium carbonate is incomplete in the prevalence of crystal during the preparation process, pattern is irregular, partial size
There is adverse effect to the processing performance and mechanical property of composite material in the problems such as wider distribution.
In order to solve above-mentioned application problem, more and more calcium carbonate manufacturers are more biased towards large-sized cubic in preparing
Winnofil, however due to the limitation of calcium carbonate crystal thermodynamics and kinetics etc., conventional carbonization method is generally difficult
To prepare the cubic winnofil that partial size is greater than 100nm, calcium carbonate crystal is only made by subsequent heat aging technique
Continued growth, to prepare big partial size winnofil, but this method takes a long time, heat consumption is higher, and preparation cost occupies high
Under not.
0447094 A1 of European patent EP discloses a kind of method for preparing the cubic winnofil of big partial size, mainly
Sodium hydroxide is first added in calcium carbonate serosity, then reheats curing.The technology effectively improves curing effect and ripe really
Change efficiency, but amount of cure tends not to stability contorting, with the introducing of alkaline matter, causes finished product pH value to increase, influence it
In filling-modified effect of rubber and plastic industry, and in maturing process, calcium carbonate particle has the tendency that cohesion, and dispersibility is deteriorated.
Chinese East China University of Science Cheng Juzheng et al. is the study found that sodium bicarbonate can also effectively facilitate the curing of calcium carbonate
Process.But curing temperature can only be maintained at 50~60 DEG C, be more than after the range, cubic calcium carbonate can change slabbing carbonic acid
Calcium.Sodium bicarbonate is similar with the mechanism of sodium hydroxide, not can be effectively controlled amount of cure equally and improves particle dispersibility.
It is still lacking in conclusion preparing large-sized cubic winnofil technique at present, it is difficult to meet industry
Metaplasia produces and the integration requirement of application market.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of high-efficient, size tunables of curing, and the calcium carbonate prepared
Particle soilless sticking trend, good dispersion the cubic winnofil of big partial size preparation method.
In order to solve the above technical problems, the technical scheme is that a kind of system of the cubic winnofil of big partial size
Preparation Method, comprising the following steps:
Step 1: lime milk density is adjusted to 1.050~1.065, temperature tune after milk of lime purification, 36~48h of ageing
Whole is 15~20 DEG C, then will be delivered in the carburizing reagent kettle with agitating function；
Step 2: being passed through purification, limekiln kiln gas after cooling into carburizing reagent kettle, make milk of lime in carburizing reagent kettle
Interior carry out carbonation reaction, the feeding flow of kiln gas are 800~1500m3/ min, carbon dioxide volume content in the kiln gas of limekiln
It is 25~35%, when reaction system conductivity is down to 0.5ms/cm, stops carburizing reagent, the specific surface area of gained calcium carbonate
(BET) between 25~45m2Between/g；
Step 3: the compound of calcium carbonate dry weight 0.3~1.0% is added in the resulting calcium carbonate serosity of step 2
Type organic metal screener stirs 20~40min, then heat aging, and 1~4h, weight are kept in 55~90 DEG C of temperature ranges
It newly is passed through limekiln kiln gas, until reaction system reaches carbonization terminal；
Step 4: the surface of calcium carbonate dry weight 2.0~5.0% is added in the resulting calcium carbonate serosity of step 3
Inorganic agent, 30~60min of stirring complete surface treatment, then successively carry out filter-press dehydration, dry, are crushed and classified to get big
The cubic winnofil of partial size.
As a preferred technical solution, the following steps are included:
Step 1: lime milk density is adjusted to 1.060, temperature is adjusted to 18 DEG C, so after milk of lime purification, ageing 40h
It will be delivered in the carburizing reagent kettle with agitating function afterwards；
Step 2: being passed through purification, limekiln kiln gas after cooling into carburizing reagent kettle, make milk of lime in carburizing reagent kettle
Interior carry out carbonation reaction, the feeding flow of kiln gas are 1200m3/ min, carbon dioxide volume content is in the kiln gas of limekiln
30%, when reaction system conductivity is down to 0.5ms/cm, stop carburizing reagent, the specific surface area (BET) of gained calcium carbonate is
32.1m2/g；
Step 3: the compound organic of calcium carbonate dry weight 0.5% is added in the resulting calcium carbonate serosity of step 2
Metallic shielding agent stirs 30min, then heat aging, keeps 1h in 80 DEG C of temperature ranges, is passed through limekiln kiln gas again,
Until reaction system reaches carbonization terminal；
Step 4: the surface treatment of calcium carbonate dry weight 2.5% is added in the resulting calcium carbonate serosity of step 3
Agent, stirring 60min complete surface treatment, then successively carry out filter-press dehydration, dry, are crushed and classified to get big partial size cube
Shape winnofil.
The compound organic metal screener is cupral and second as a preferred technical solution,
The mixture of the big sodium acetate of two salicyl of diamines.
The cupral and the big second of two salicyl of ethylenediamine as a preferred technical solution,
The mixed proportion of sour sodium is 1:1~3:1.
The surface treating agent includes fatty acid or fatty acid sodium salt as a preferred technical solution,.
The fatty acid sodium salt includes odium stearate as a preferred technical solution,
The carbonization terminal refers to reaction system pH≤7.5 as a preferred technical solution,.
The volume of the carburizing reagent kettle is 50 cubic metres as a preferred technical solution, and the carburizing reagent kettle is filled out
Filling coefficient is 0.65~0.85.
As improvement to above-mentioned technical proposal, the particle size range of the big cubic winnofil of partial size is 165~
300nm。
By adopting the above-described technical solution, the invention has the following advantages that
1, made from the traditional heating ageing method compared with winnofil, technique curing of the present invention is high-efficient,
The cubic winnofil of big partial size can be obtained within a short period of time；
2, compared with sodium hydroxide or sodium bicarbonate accelerate ageing method, the winnofil of present invention process preparation is utilized
Dispersibility is excellent, reunites few, and size tunable；
3, present invention process simple possible, production cost is low, has preferable economic benefit.
Detailed description of the invention
The following drawings are only intended to schematically illustrate and explain the present invention, not delimit the scope of the invention.Wherein:
Fig. 1 is the electron scanning micrograph that the cubic winnofil of big partial size is made in the embodiment of the present invention；
Fig. 2 is the electron scanning micrograph that winnofil is made in the prior art.
Specific embodiment
With reference to the accompanying drawings and examples, the present invention is further explained.In the following detailed description, only pass through explanation
Mode describes certain exemplary embodiments of the invention.Undoubtedly, those skilled in the art will recognize, In
In the case where without departing from the spirit and scope of the present invention, described embodiment can be repaired with a variety of different modes
Just.Therefore, attached drawing and description are regarded as illustrative in nature, and are not intended to limit the scope of the claims.
The invention discloses a kind of preparation methods of big cubic winnofil of partial size, comprising the following steps:
Step 1: lime milk density is adjusted to 1.050~1.065, temperature tune after milk of lime purification, 36~48h of ageing
Whole is 15~20 DEG C, then will be delivered in the carburizing reagent kettle with agitating function.The volume of the carburizing reagent kettle is 50
Cubic meter, the filling coefficient of the carburizing reagent kettle are 0.65~0.85.
Step 2: being passed through purification, limekiln kiln gas after cooling into carburizing reagent kettle, make milk of lime in carburizing reagent kettle
Interior carry out carbonation reaction, the feeding flow of kiln gas are 800~1500m3/ min, carbon dioxide volume content in the kiln gas of limekiln
It is 25~35%, when reaction system conductivity is down to 0.5ms/cm, stops carburizing reagent, the specific surface area of gained calcium carbonate
(BET) between 25~45m2Between/g.
Step 3: the compound of calcium carbonate dry weight 0.3~1.0% is added in the resulting calcium carbonate serosity of step 2
Type organic metal screener stirs 20~40min, then heat aging, and 1~4h, weight are kept in 55~90 DEG C of temperature ranges
It newly is passed through limekiln kiln gas, until reaction system reaches carbonization terminal, the carbonization terminal refers to reaction system pH≤7.5.
Step 4: the surface of calcium carbonate dry weight 2.0~5.0% is added in the resulting calcium carbonate serosity of step 3
Inorganic agent, 30~60min of stirring complete surface treatment, then successively carry out filter-press dehydration, dry, are crushed and classified to get big
The cubic winnofil of partial size.
Compound organic metal screener described in step 3 is cupral and the adjacent hydroxyl of ethylenediamine two
The mixture of the big sodium acetate of phenyl, and the cupral and the big sodium acetate of two salicyl of ethylenediamine
Mixed proportion be 1:1~3:1.The surface treating agent includes fatty acid or fatty acid sodium salt, wherein the fatty acid sodium salt
Including odium stearate.
By adjusting a technological parameter, the big cubic precipitating carbonic acid of partial size made from the above method through the invention
The particle size range of calcium is 165~300nm.The invention is described in detail below by specific embodiment.
Embodiment one:
During the preparation process, the parameter of use is as described below for the present embodiment:
Step 1: lime milk density is adjusted to 1.050, temperature is adjusted to 15 DEG C, so after milk of lime purification, ageing 40h
It will be delivered in the carburizing reagent kettle with agitating function afterwards, the volume of the carburizing reagent kettle is 50 cubic metres, the carbonization
The filling coefficient of reaction kettle is 0.75.
Step 2: being passed through purification, limekiln kiln gas after cooling into carburizing reagent kettle, make milk of lime in carburizing reagent kettle
Interior carry out carbonation reaction, the feeding flow of kiln gas are 1200m3/ min, carbon dioxide volume content is in the kiln gas of limekiln
30%, when reaction system conductivity is down to 0.5ms/cm, stop carburizing reagent, the specific surface area (BET) of gained calcium carbonate is
43.7m2/g。
Step 3: the compound organic of calcium carbonate dry weight 1.0% is added in the resulting calcium carbonate serosity of step 2
Metallic shielding agent stirs 30min, then heat aging, keeps 1h in 90 DEG C of temperature ranges, is passed through limekiln kiln gas again,
Until reaction system reaches carbonization terminal, the carbonization terminal refers to reaction system pH≤7.5, described compound in this step
The cupral that organic metal screener uses and the big sodium acetate of two salicyl of ethylenediamine
Mixed proportion is 2:1.
Step 4: the odium stearate of calcium carbonate dry weight 2.0% is added in the resulting calcium carbonate serosity of step 3,
It stirs 60min and completes surface treatment, then successively carry out filter-press dehydration, dry, be crushed and classified and sink to get big partial size is cubic
Shallow lake calcium carbonate, by the parameter setting in the embodiment, the partial size of the big cubic winnofil of partial size obtained is 285nm,
Pattern is stereo structure.
Embodiment two:
During the preparation process, the parameter of use is as described below for the present embodiment:
Step 1: lime milk density is adjusted to 1.060, temperature is adjusted to 18 DEG C, so after milk of lime purification, ageing 40h
It will be delivered in the carburizing reagent kettle with agitating function afterwards, the volume of the carburizing reagent kettle is 50 cubic metres, the carbonization
The filling coefficient of reaction kettle is 0.75.
Step 2: being passed through purification, limekiln kiln gas after cooling into carburizing reagent kettle, make milk of lime in carburizing reagent kettle
Interior carry out carbonation reaction, the feeding flow of kiln gas are 1200m3/ min, carbon dioxide volume content is in the kiln gas of limekiln
30%, when reaction system conductivity is down to 0.5ms/cm, stop carburizing reagent, the specific surface area (BET) of gained calcium carbonate is
32.4m2/g。
Step 3: the compound organic of calcium carbonate dry weight 0.6% is added in the resulting calcium carbonate serosity of step 2
Metallic shielding agent stirs 30min, then heat aging, keeps 1h in 80 DEG C of temperature ranges, is passed through limekiln kiln gas again,
Until reaction system reaches carbonization terminal, the carbonization terminal refers to reaction system pH≤7.5, described compound in this step
The cupral that organic metal screener uses and the big sodium acetate of two salicyl of ethylenediamine
Mixed proportion is 3:1.
Step 4: the odium stearate of calcium carbonate dry weight 2.5% is added in the resulting calcium carbonate serosity of step 3,
It stirs 60min and completes surface treatment, then successively carry out filter-press dehydration, dry, be crushed and classified and sink to get big partial size is cubic
Shallow lake calcium carbonate, by the parameter setting in the embodiment, the partial size of the big cubic winnofil of partial size obtained is 190nm,
Pattern is stereo structure.
Embodiment three:
During the preparation process, the parameter of use is as described below for the present embodiment:
Step 1: lime milk density is adjusted to 1.065, temperature is adjusted to 18 DEG C, so after milk of lime purification, ageing 40h
It will be delivered in the carburizing reagent kettle with agitating function afterwards, the volume of the carburizing reagent kettle is 50 cubic metres, the carbonization
The filling coefficient of reaction kettle is 0.75.
Step 2: being passed through purification, limekiln kiln gas after cooling into carburizing reagent kettle, make milk of lime in carburizing reagent kettle
Interior carry out carbonation reaction, the feeding flow of kiln gas are 1200m3/ min, carbon dioxide volume content is in the kiln gas of limekiln
30%, when reaction system conductivity is down to 0.5ms/cm, stop carburizing reagent, the specific surface area (BET) of gained calcium carbonate is
32.1m2/g。
Step 3: the compound organic of calcium carbonate dry weight 0.5% is added in the resulting calcium carbonate serosity of step 2
Metallic shielding agent stirs 30min, then heat aging, keeps 1h in 80 DEG C of temperature ranges, is passed through limekiln kiln gas again,
Until reaction system reaches carbonization terminal, the carbonization terminal refers to reaction system pH≤7.5, described compound in this step
The cupral that organic metal screener uses and the big sodium acetate of two salicyl of ethylenediamine
Mixed proportion is 2:1.
Step 4: the odium stearate of calcium carbonate dry weight 2.5% is added in the resulting calcium carbonate serosity of step 3,
It stirs 60min and completes surface treatment, then successively carry out filter-press dehydration, dry, be crushed and classified and sink to get big partial size is cubic
Shallow lake calcium carbonate, by the parameter setting in the embodiment, the partial size of the big cubic winnofil of partial size obtained is 165nm,
Pattern is stereo structure.
Comparative example 1:
As shown in Fig. 2, using sodium hydroxide, calcium carbonate product made from the preparation method according to the prior art is averaged
Partial size is 95nm, and pattern is that class is cubic, and dispersibility is poor.
Shown in Fig. 1, to utilize the cubic winnofil of big partial size made from embodiment 1, by that can be seen compared with Fig. 2
Out, the winnofil dispersibility prepared using present invention process is excellent, reunites few, and can be with by embodiment 1 to embodiment 3
Find out, by adjusting technological parameter the cubic winnofil of big partial size of different-grain diameter can be made, therefore in present invention process
The cubic winnofil size tunable of big partial size produced by the present invention, and present invention process simple possible, production cost is low, tool
There is preferable economic benefit.
The above shows and describes the basic principle, main features and advantages of the invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (6)
1. a kind of preparation method of the cubic winnofil of big partial size, which comprises the following steps:
Step 1: lime milk density is adjusted to 1.050~1.065, temperature is adjusted to after milk of lime purification, 36~48h of ageing
It 15~20 DEG C, then will be delivered in the carburizing reagent kettle with agitating function；
Step 2: be passed through purification, limekiln kiln gas after cooling into carburizing reagent kettle, make milk of lime in carburizing reagent kettle into
Row carbonation reaction, the feeding flow of kiln gas are 800~1500m3/ min, carbon dioxide volume content is 25 in the kiln gas of limekiln
~35%, when reaction system conductivity is down to 0.5ms/cm, stop carburizing reagent, the specific surface area (BET) of gained calcium carbonate
Between 25~45m2Between/g；
Step 3: the compound of calcium carbonate dry weight 0.3~1.0%, which is added, to be had in the resulting calcium carbonate serosity of step 2
Machine metallic shielding agent stirs 20~40min, then heat aging, and 1~4h is kept in 55~90 DEG C of temperature ranges, is led to again
Enter limekiln kiln gas, until reaction system reaches carbonization terminal；
The compound organic metal screener is cupral and the big sodium acetate of two salicyl of ethylenediamine
Mixture；
Step 4: the surface treatment of calcium carbonate dry weight 2.0~5.0% is added in the resulting calcium carbonate serosity of step 3
Agent, 30~60min of stirring complete surface treatment, then successively carry out filter-press dehydration, dry, are crushed and classified to get big partial size
Cubic winnofil；
The particle size range of the cubic winnofil of big partial size is 165~300nm.
2. a kind of preparation method of the big cubic winnofil of partial size as described in claim 1, which is characterized in that including with
Lower step:
Step 1: lime milk density is adjusted to 1.060 after milk of lime purification, ageing 40h, temperature is adjusted to 18 DEG C, then will
It is delivered in the carburizing reagent kettle with agitating function；
Step 2: be passed through purification, limekiln kiln gas after cooling into carburizing reagent kettle, make milk of lime in carburizing reagent kettle into
Row carbonation reaction, the feeding flow of kiln gas are 1200m3/ min, carbon dioxide volume content is 30% in the kiln gas of limekiln, when
When reaction system conductivity is down to 0.5ms/cm, stop carburizing reagent, the specific surface area (BET) of gained calcium carbonate is 32.1m2/
g；
Step 3: the compound organic metal of calcium carbonate dry weight 0.5% is added in the resulting calcium carbonate serosity of step 2
Screener stirs 30min, then heat aging, keeps 1h in 80 DEG C of temperature ranges, is passed through limekiln kiln gas again, until
Reaction system reaches carbonization terminal；
Step 4: the surface treating agent of calcium carbonate dry weight 2.5% is added, stirs in the resulting calcium carbonate serosity of step 3
It mixes 60min and completes surface treatment, then successively carry out filter-press dehydration, dry, be crushed and classified to get the cubic precipitating of big partial size
Calcium carbonate.
3. a kind of preparation method of the big cubic winnofil of partial size as claimed in claim 1 or 2, which is characterized in that institute
The mixed proportion for stating cupral and the big sodium acetate of two salicyl of ethylenediamine is 1:1~3:1.
4. a kind of preparation method of the big cubic winnofil of partial size as claimed in claim 1 or 2, which is characterized in that institute
Stating surface treating agent includes fatty acid.
5. a kind of preparation method of the big cubic winnofil of partial size as claimed in claim 1 or 2, which is characterized in that institute
It states carbonization terminal and refers to reaction system pH≤7.5.
6. a kind of preparation method of the big cubic winnofil of partial size as claimed in claim 1 or 2, which is characterized in that institute
The volume for stating carburizing reagent kettle is 50 cubic metres, and the filling coefficient of the carburizing reagent kettle is 0.65~0.85.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711261405.0A CN107827137B (en) | 2017-12-04 | 2017-12-04 | A kind of preparation method of the cubic winnofil of big partial size |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711261405.0A CN107827137B (en) | 2017-12-04 | 2017-12-04 | A kind of preparation method of the cubic winnofil of big partial size |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107827137A CN107827137A (en) | 2018-03-23 |
| CN107827137B true CN107827137B (en) | 2019-11-12 |
Family
ID=61641400
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711261405.0A Active CN107827137B (en) | 2017-12-04 | 2017-12-04 | A kind of preparation method of the cubic winnofil of big partial size |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107827137B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650431A (en) * | 2019-01-07 | 2019-04-19 | 卢氏国嵩莱纳米科技有限公司 | A kind of preparation method of MS glue nanometer calcium carbonate |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1817796A (en) * | 2006-01-16 | 2006-08-16 | 同济大学 | Control of shape and appearance of calcium carbonate |
| CN103663527B (en) * | 2012-09-25 | 2016-02-10 | 上海华明高技术（集团）有限公司 | The preparation method of cubic ultra-fine calcium carbonate particle |
| CN103508479A (en) * | 2013-10-22 | 2014-01-15 | 山西兰花华明纳米材料有限公司 | Production method of nanometer calcium carbonate for electronic glue |
| CN104609453B (en) * | 2014-11-25 | 2016-08-24 | 广西华纳新材料科技有限公司 | A kind of preparation method of cubic winnofil |
-
2017
- 2017-12-04 CN CN201711261405.0A patent/CN107827137B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN107827137A (en) | 2018-03-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105836781B (en) | A kind of carbonization-activation integrated apparatus and method for producing nano-calcium carbonate | |
| CN106517285B (en) | A kind of preparation method of rod-like nano calcium carbonate | |
| KR101196041B1 (en) | Process for production of pcc | |
| CN101774623B (en) | Industrial preparation method of rice-shaped ultra-fine activated calcium carbonate | |
| CN100450932C (en) | Nm-class calcium carbonate carbonization process | |
| CA2290816C (en) | Seeding of aragonite calcium carbonate and the product thereof | |
| CN105482500B (en) | The surface modifying method of silicone sealant antioxidant nano-calcium carbonate | |
| CN104893361B (en) | The Nano calcium carbonate dedicated preparation method of sealing neutral silicone resin | |
| CN103665937B (en) | Method for preparing nano calcium carbonate specially used for middle and top grade silicone sealants | |
| CN111268712A (en) | Method for preparing nano calcium carbonate by using crystal form control agent for regulation and control | |
| CN106276931B (en) | A kind of microwave synthesis method of lithium magnesium silicate | |
| CN102701255A (en) | Method for high-concentration carbonization production of spherical nano calcium carbonate | |
| CN1429772A (en) | Method for preparing calcium carbonate with actual forms | |
| CN104403433B (en) | The preparation method of the special winnofil of PVC stone-impact-proof paint | |
| CN101585976A (en) | Low-viscosity active calcium carbonate, preparation method and application thereof | |
| CN103693667A (en) | Rodlike light calcium carbonate and preparation method thereof | |
| CN107724171A (en) | A kind of Nano calcium carbonate dedicated preparation method of papermaking | |
| CN106830041B (en) | A kind of preparation method of functional calcium carbonate | |
| CN106634049A (en) | Method for preparing nano calcium carbonate for weather-resistant ink | |
| FI105545B (en) | Precipitated calcium carbonate | |
| CN104479411A (en) | Surface modification method of special nano calcium carbonate for silicone sealants | |
| CN105836782B (en) | calcite type calcium carbonate and preparation method thereof | |
| CN107827137B (en) | A kind of preparation method of the cubic winnofil of big partial size | |
| CN108439450A (en) | A kind of preparation method of nano-calcium carbonate for building | |
| CN104609453B (en) | A kind of preparation method of cubic winnofil |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation of cubic precipitated calcium carbonate with large particle size Effective date of registration: 20201130 Granted publication date: 20191112 Pledgee: Qingzhou Jinding sub branch of Weifang Bank Co.,Ltd. Pledgor: QINGZHOU YUXIN CALCIUM INDUSTRIAL Co.,Ltd. Registration number: Y2020980008603 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20220915 Granted publication date: 20191112 Pledgee: Qingzhou Jinding sub branch of Weifang Bank Co.,Ltd. Pledgor: QINGZHOU YUXIN CALCIUM INDUSTRIAL CO.,LTD. Registration number: Y2020980008603 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221208 Address after: 262503 Dianzi Industrial Park, Miaozi Town, Weifang City, Shandong Province Patentee after: Shandong Yuxin Nano Technology Co.,Ltd. Address before: 262503 nanzhudian village, Miaozi Town, Qingzhou City, Weifang City, Shandong Province Patentee before: QINGZHOU YUXIN CALCIUM INDUSTRIAL CO.,LTD. |
|
| TR01 | Transfer of patent right |