AU2021105679A4 - Modification Method of Silica Polymer Coating - Google Patents
Modification Method of Silica Polymer Coating Download PDFInfo
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- AU2021105679A4 AU2021105679A4 AU2021105679A AU2021105679A AU2021105679A4 AU 2021105679 A4 AU2021105679 A4 AU 2021105679A4 AU 2021105679 A AU2021105679 A AU 2021105679A AU 2021105679 A AU2021105679 A AU 2021105679A AU 2021105679 A4 AU2021105679 A4 AU 2021105679A4
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- AU
- Australia
- Prior art keywords
- polymer coating
- modification method
- reaction kettle
- coating modification
- suspension
- 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.)
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 34
- 239000011248 coating agent Substances 0.000 title claims abstract description 21
- 238000000576 coating method Methods 0.000 title claims abstract description 21
- 229920000642 polymer Polymers 0.000 title claims abstract description 21
- 238000002715 modification method Methods 0.000 title claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- 239000000725 suspension Substances 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003607 modifier Substances 0.000 claims abstract description 17
- 239000000839 emulsion Substances 0.000 claims abstract description 16
- 239000006229 carbon black Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 8
- 235000007164 Oryza sativa Nutrition 0.000 claims abstract description 7
- 239000002956 ash Substances 0.000 claims abstract description 7
- 239000010903 husk Substances 0.000 claims abstract description 7
- 235000009566 rice Nutrition 0.000 claims abstract description 7
- 240000007594 Oryza sativa Species 0.000 claims abstract 2
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 19
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 238000001556 precipitation Methods 0.000 abstract description 4
- 239000011265 semifinished product Substances 0.000 abstract description 3
- 238000006011 modification reaction Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 241000209094 Oryza Species 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229940037003 alum Drugs 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 210000003205 muscle Anatomy 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 2
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 101001012040 Pseudomonas aeruginosa (strain ATCC 15692 / DSM 22644 / CIP 104116 / JCM 14847 / LMG 12228 / 1C / PRS 101 / PAO1) Immunomodulating metalloprotease Proteins 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3072—Treatment with macro-molecular organic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a white carbon black polymer coating modification method,
which is carried out according to the following steps: step 1, rice husk ash, sodium silicate and
sulfuric acid are precipitated and reacted to obtain a suspension, and the suspension is put into
a modification reaction kettle; Adding wax emulsion into the reaction kettle; 3, the reaction is
completed after stirring; Adding a modifier into the reaction kettle; Step 5, after cooling, the
mixed hydraulic pressure in the reaction kettle is filtered and washed clean; Step 6, drying to
obtain coated modified white carbon black. The invention has the beneficial effects that: By
adding wax emulsion into the suspension after precipitation reaction of sodium silicate and
sulfuric acid, The modified silica can be modified by adding modifier into the suspension after
the precipitation reaction. The main characteristics of this method are simple process and few
auxiliary equipment, which can modify the precipitated silica, especially the semi-finished
product of precipitated silica, and is beneficial to reduce the product cost.
Description
Modification Method of Silica Polymer Coating
The invention relates to a white carbon black polymer coating modification
method, belonging to the technical field of white carbon black modification.
At present, the silica prepared by traditional methods has large particle size.
Moreover, due to the existence of a large number of active silica hydroxyl groups on the
surface of nano-silica, the surface of nano-silica is hydrophilic and oleophobic, easy to
reunite, difficult to infiltrate and disperse in organic media, and difficult to play its role
when directly filled into organic materials, which limits the industrial application of
nano-silica. Therefore, it is necessary to modify the surface of silica, weaken the
polarity of silica surface and reduce the energy state of silica surface, so as to improve
the compatibility between nanoparticles and organic matrix, improve its application
effect, increase the added value of products and expand the application fields of
products.
The technical problem to be solved by the invention is to provide a silica polymer
coating modification method, which is mainly characterized by simple process and few
auxiliary equipment, can modify precipitated silica, especially semi-finished products
of precipitated silica, and is beneficial to reduce product cost.
The invention is realized by the following scheme: a white carbon black polymer
coating modification method, which is carried out according to the following steps:
Step 1.The rice husk ash, sodium silicate and sulfuric acid are precipitated and
reacted to obtain a suspension, and the suspension is put into a modified reaction kettle;
Step 2.Adding wax emulsion into the reaction kettle;
Step 3.the reaction is completed after stirring;
Step 4.Adding a modifier into the reaction kettle;
Step 5, after cooling, the mixed hydraulic pressure in the reaction kettle is filtered
and washed clean;
Step 6, drying to obtain coated modified white carbon black.
The invention discloses a method for coating and modifying white carbon black
polymer, which is carried out according to the following steps:
Step 1.The rice husk ash, sodium silicate and sulfuric acid are precipitated and
reacted to obtain a suspension, and the suspension is placed into a modified reaction
kettle;
Step 2.Adding wax emulsion into the reaction kettle;
Step 3. the reaction is completed after pressurizing, stirring and heating;
Step 4.Adding a modifier into the reaction kettle, heating and stirring;
Step 5.after cooling, the mixed hydraulic pressure in the reaction kettle is filtered
and washed clean through a dynamic washing tank;
Step 6, drying by a rotary flash dryer to obtain coated modified white carbon
black.
The volume ratio of the suspension to the wax emulsion in the step 2 is 5-6: 1.
In the third step, the pressure is pressurized to 0.8-IMPa.
The stirring rate in the third step is 50-70r/min.
The heating temperature in the third step is 200-220°C.
The reaction time of the third step is 4-6h.
Stirring for 4-6h at a stirring rate of 30r/min at a controlled temperature of82-96°C
in step 4;
The drying time in the step 6 is 2h-4h.
In the sixth step, the inlet temperature of the hot air is controlled to be 400-500°C,
and the outlet temperature of the tail gas is 150-200°C.
The invention has the beneficial effects that:
1. The invention relates to a silica polymer coating modification method by
adding wax emulsion into the suspension after the precipitation reaction of sodium
silicate and sulfuric acid, The modified silica can be modified by adding modifier into
the suspension after the precipitation reaction. The main characteristics of this method
are simple process and few auxiliary equipment, which can modify the precipitated
silica, especially the semi-finished product of precipitated silica, and is beneficial to
reduce the product cost.
The present invention is further described below, but the scope of protection of the
present invention is not limited to the above contents.
For clarity, Without describing all the features of the actual embodiment, In the
following description, Without describing well-known functions and structures in
detail, Because they confuse the invention with unnecessary details, It should be considered that in the development of any actual embodiment, A great deal of implementation detail must be made to achieve the specific goals of the developer, such as changing from one embodiment to another in accordance with system-related or business-related limitations. In addition, it should be considered that such development work may be complex and time-consuming, but is only routine work for those skilled in the art.
Example 1: A silica polymer coating modification method, which is carried out
according to the following steps:
Step 1,The rice husk ash, sodium silicate and sulfuric acid are precipitated and
reacted to obtain a suspension, and the suspension is placed into a modified reaction
kettle;
Step 2, Adding wax emulsion into the reaction kettle, wherein the volume ratio of
the suspension to the wax emulsion is 5: 1;
Step 3, pressurizing to 0.8 MPa, heating to 200°C at stirring rate of 50r/min, and
completing the reaction after 4 hours;
Step 4, Adding a modifier into the reaction kettle, controlling the temperature to
82 °C, and stirring for 4 hours at a stirring rate of 30r/min;
Step 5, after cooling, the mixed hydraulic pressure in the reaction kettle is filtered
and washed clean through a dynamic washing tank;
Step 6, drying by a rotary flash dryer, controlling the drying time for 2hh, the inlet
temperature of hot air at 400°C, and the outlet temperature of tail gas at 150°C to obtain
the coated modified silica.
Example 2: A silica polymer coating modification method, which is carried out
according to the following steps:
Step 1,The rice husk ash, sodium silicate and sulfuric acid are precipitated and
reacted to obtain a suspension, and the suspension is placed into a modified reaction
kettle;
Step 2,Adding wax emulsion into the reaction kettle, wherein the volume ratio of
the suspension to the wax emulsion is 6: 1;
Step 3, pressurizing to IMPa, heating to 220°C at a stirring rate of 70r/min, and
completing the reaction after 6h;
Step 4,Adding modifier into the reaction kettle, controlling the temperature to
96 °Cand stirring for 6 hours at the stirring rate of 30r/min;
Step 5, after cooling, the mixed hydraulic pressure in the reaction kettle is filtered
and washed clean through a dynamic washing tank;
Step 6, drying by a rotary flash dryer, controlling the drying time for 4h, the inlet
temperature of hot air 500°C, and the outlet temperature of tail gas 200°C to obtain the
coated modified white carbon black.
Example 3: A silica polymer coating modification method, which is carried out
according to the following steps:
Step 1,The rice husk ash, sodium silicate and sulfuric acid are precipitated and
reacted to obtain a suspension, and the suspension is placed into a modified reaction
kettle;
Step 2,Adding wax emulsion into the reaction kettle, wherein the volume ratio of
the suspension to the wax emulsion is 5.5: 1;
Step 3, pressurizing to 0.9 MPa, heating to 210°C at stirring rate of 60r/min, and
completing the reaction after 5 hours;
Step 4.Adding modifier into the reaction kettle, controlling the temperature to
°C and stirring for 5 hours at the stirring rate of 30r/min;
Step 5, after cooling, the mixed hydraulic pressure in the reaction kettle is filtered
and washed clean through a dynamic washing tank;
Step 6, Drying by a rotary flash dryer, controlling the drying time for 3 hours, the
inlet temperature of hot air is 450°C, and the outlet temperature of tail gas is 180°C, so
as to obtain the coated modified white carbon black.
Effect of modifier types and dosage on specific surface area of silica products.
Specific surface area is defined as the surface area per unit powder mass in in2/g or
cm2/g. Specific surface area is one of the most important surface properties of powder
materials, and it is also one of the main basis for determining the amount of surface
modifiers. The classification of precipitated silica is defined in Appendix E of the
international standard IS05974-1: 1994 (the standard HG/T3061-1999 is equivalent).
The classification is classified into A, B, C, D, E and F6 according to the specific
surface area of nitrogen adsorption (m2/g), and their corresponding ranges are > 191,
161 ~ 190, 136-'160, 106 ~ 135, 71 ~ 105 and < 7013 respectively. The specific surface
area of silica reflects the size of its primary particles, which is the main index affecting
its application performance. Generally speaking, the larger the specific surface area of silica, the better the reinforcing effect in rubber. However, when the specific surface area is too large, the cohesion between particles is enhanced, and it is not easy to disperse in the compound, which makes the compound have high viscosity, high heat generation and easy scorch during processing. Therefore, the processing unit requires silica manufacturers to provide various brands of products with different specific surface areas to meet the reinforcement needs of different products HI. Before acid precipitation, five kinds of modifiers with different dosages were added to obtain different modified silica products, and their specific surface areas were measured. The results are shown in the following table.
It can be seen from the table that when using wax emulsion, the product has a
larger specific surface area in all modified products with the same amount, especially
when the amount of modifier is greater than%, the specific surface area of the product is
greater than 200m2/g, and the maximum value is 271.105 m2/g, which is obtained
when using alum A-189 for modification. When the amount of vinylsilane A-151 and
aminosilane KH-550 is constant, the specific surface area of the product also exceeds
200m2/g. When nonionic surfaces are used, it can be seen from the table that when wax
emulsion is used, the specific surface area of the products obtained is larger than
200m2/g, especially when the amount of modifier is greater than%, and the maximum
value is 271.105 m2/g, which is obtained when alum A-189 is used for modification.
When the amount of vinylsilane A-151 and aminosilane KH-550 is constant, the
specific surface area of the product also exceeds 200m2/g. When the nonionic
surfactant OP-10 is used as modifier, the specific surface area of the product is smaller than that of other products at the same dosage. When the dosage of OP-10 is muscle, the specific surface area of silica obtained is the smallest, which is 118.078 m2/g. When the active agent OP-10 is used as modifier, the specific surface area of the product obtained is smaller than that of other products at the same dosage. When the dosage of OP-10 is muscle, the specific surface area of silica obtained is the smallest, which is 118.078 m2/g.
Although the technical scheme of the present invention has been described and
enumerated in detail, It will be understood that it will be apparent to those skilled in the
art that modifications or equivalent alternatives to the above-described embodiments
are made and that such modifications or improvements made without departing from
the spirit of the invention fall within the scope of the claimed invention.
Claims (1)
- THE CLAIMS DEFINING THE INVENTION ARE AS FOLLOWS:1. A white carbon black polymer coating modification method is characterized inthat the method is carried out according to the following steps:Step 1,the rice husk ash, sodium silicate and sulfuric acid are precipitated andreacted to obtain a suspension, and the suspension is placed into a modified reactionkettle;Step 2,adding wax emulsion into the reaction kettle;Step 3, the reaction is completed after stirring;Step 4,adding a modifier into the reaction kettle;Step 5, after cooling, the mixed hydraulic pressure in the reaction kettle is filteredand washed clean;Step 6, drying to obtain coated modified white carbon black.A silica polymer coating modification method according to Claim 1, characterizedin that the method is carried out according to the following steps:Step3, the reaction is completed after pressurizing, stirring and heating;Step4,Adding a modifier into the reaction kettle, heating and stirring;Step 5, after cooling, the mixed hydraulic pressure in the reaction kettle is filteredand washed clean through a dynamic washing tank;Step 6, drying by a rotary flash dryer to obtain coated modified white carbonblack.The silica polymer coating modification method according to Claim 2 ischaracterized in that the volume ratio of the suspension to the wax emulsion in Step 2 is-6: 1.The white carbon black polymer coating modification method according to claim2 is characterized in that in the step 3, the pressure is pressurized to 0.8-iMPaThe silica polymer coating modification method according to Claim 2 ischaracterized in that the stirring rate in Step 3 is 50-70r/min.The silica polymer coating modification method according to claim 2 ischaracterized in that the heating temperature in step 3 is 200-220 °C.The silica polymer coating modification method according to Claim 2 ischaracterized in that the reaction time of the Step 3 is 4-6h.The silica polymer coating modification method according to claim 2 ischaracterized in that in the step 4, the control temperature is 82-96 °C, and the stirringrate is 30r/min for 4-6h.The white carbon black polymer coating modification method according to Claim2 is characterized in that the drying time in Step 6 is 2h-4hThe white carbon black polymer coating modification method according to claim2 is characterized in that the inlet temperature of hot air is controlled to be400-500°Cand the outlet temperature of tail gas is controlled to be 150-200 °C. in step6.FIGURES 1/1
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2021105679A AU2021105679A4 (en) | 2021-08-17 | 2021-08-17 | Modification Method of Silica Polymer Coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2021105679A AU2021105679A4 (en) | 2021-08-17 | 2021-08-17 | Modification Method of Silica Polymer Coating |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| AU2021105679A4 true AU2021105679A4 (en) | 2021-10-14 |
Family
ID=78007611
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AU2021105679A Ceased AU2021105679A4 (en) | 2021-08-17 | 2021-08-17 | Modification Method of Silica Polymer Coating |
Country Status (1)
| Country | Link |
|---|---|
| AU (1) | AU2021105679A4 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114364634A (en) * | 2021-12-01 | 2022-04-15 | 无锡恒诚硅业有限公司 | Preparation method and application of white carbon black for coating |
| CN115159534A (en) * | 2022-08-15 | 2022-10-11 | 湖北新蓝天新材料股份有限公司 | Surface modification method of precipitated white carbon black |
-
2021
- 2021-08-17 AU AU2021105679A patent/AU2021105679A4/en not_active Ceased
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114364634A (en) * | 2021-12-01 | 2022-04-15 | 无锡恒诚硅业有限公司 | Preparation method and application of white carbon black for coating |
| WO2023097544A1 (en) * | 2021-12-01 | 2023-06-08 | 无锡恒诚硅业有限公司 | Preparation method for white carbon black for coating and application |
| CN115159534A (en) * | 2022-08-15 | 2022-10-11 | 湖北新蓝天新材料股份有限公司 | Surface modification method of precipitated white carbon black |
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| Date | Code | Title | Description |
|---|---|---|---|
| FGI | Letters patent sealed or granted (innovation patent) | ||
| MK22 | Patent ceased section 143a(d), or expired - non payment of renewal fee or expiry |