CN104448935A - Preparation method for nano-calcium carbonate composite particle - Google Patents
Preparation method for nano-calcium carbonate composite particle Download PDFInfo
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- CN104448935A CN104448935A CN201310417773.5A CN201310417773A CN104448935A CN 104448935 A CN104448935 A CN 104448935A CN 201310417773 A CN201310417773 A CN 201310417773A CN 104448935 A CN104448935 A CN 104448935A
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Abstract
Belonging to the technical field of nano-material preparation, the invention relates to a preparation method for a nano-calcium carbonate composite particle, in particular to preparation of the nano-calcium carbonate composite particle by an emulsion polymerization method. The invention provides the method preparation of the nano-calcium carbonate composite particle by the emulsion polymerization process. The method includes: firstly employing MPTMS accounting for 3.5% of nano-calcium carbonate to conduct ultrasonic dispersion in toluene medium to conduct pretreatment, and carrying out pumping filtration, drying and grinding; then adding metered SDS, distilled water and surface pretreated nano C bing 3 into a three-neck bottle, adjusting the pH to 8-9 with ammonia water, conducting ultrasonic dispersion for 5-10min, then raising the temperature and conducting stirring, under a temperature of 55-80DEG C adding a KPS solution, slowly adding BA and MMA successively in stages by a "starvation" technique, carrying out reaction at 70DEG C for 7h, and carrying out after-treatment so as to obtain the nano-calcium carbonate polymer composite particle.
Description
Technical field
the invention belongs to the preparing technical field of nano material, specifically, the present invention relates to emulsion polymerization and prepare nano-calcium carbonate composite particles.
Background technology
the activeness and quietness appearing as polymkeric substance has opened up new development space, but its surface energy is high, hydrophilic oleophobic, with superpolymer poor compatibility, disperses bad in the base.For this reason, adopt suitable surface treatment means to reduce nano-calcium carbonate surface polarity, improve its dispersiveness in polymeric matrix and be the toughness reinforcing matter of utmost importance that will solve of enhancing by polymer with the consistency of matrix.With polymkeric substance, the consistency that coated process can improve inorganic particulate and matrix is carried out to inorganic particulate, promote filler dispersion in the base, thus favored.In numerous polymer overmold treatment processs, emulsion polymerization is comparatively ripe, is successfully applied to Ti0
2
, Si0
2
, CaC0
3
etc. the surface treatment of multiple inorganic particulate, but the research report adopting dual MCU system letex polymerization to carry out modification to inorganic particulate is relatively less.
Summary of the invention
the present invention is exactly for the problems referred to above, provides a kind of method that emulsion polymerization prepares nano-calcium carbonate composite particles.
for realizing above-mentioned purpose of the present invention, the present invention adopts following technical scheme, and the present invention adopts method as follows: first use the MPTMS of nano-calcium carbonate 3.5% in toluene medium under ultrasonic disperse to its pre-treatment, suction filtration, dry, grinding.The SDS of metering, distilled water and through the nanometer C of surface preparation bright 3 is added in there-necked flask, pH to 8 ~ 9 are adjusted with ammoniacal liquor, heat up after ultrasonic disperse 5 ~ 10 min, stir, KPS solution is added when 55 ~ 80 DEG C, " starvation method " successively segmentation is adopted slowly to add BA and MMA, 70 DEG C of reaction 7 h, obtain nano-calcium carbonate polymer composite particle through aftertreatment.
beneficial effect of the present invention:
(1) adopt MPTMS pre-treatment, CaO monomer=I/0.5, SDS consumption slightly larger than CMC, adjust pH=8 ~ 9, substep feeding mode carries out letex polymerization, can obtain finely disseminated polymer overmold nanometer CaC0
3
composite particles.
(2) FT-IR shows, P (BA-co-MMA) is coated on nanometer CaC0 with bonding pattern
3
surface.
(3) contact angle and settling volume data show, polymer overmold process nanometer CaC0
3
polarity and surface tension significantly reduce.
Embodiment
the present invention adopts method as follows: first use the MPTMS of nano-calcium carbonate 3.5% in toluene medium under ultrasonic disperse to its pre-treatment, suction filtration, dry, grinding.The SDS of metering, distilled water and through the nanometer C of surface preparation bright 3 is added in there-necked flask, pH to 8 ~ 9 are adjusted with ammoniacal liquor, heat up after ultrasonic disperse 5 ~ 10 min, stir, KPS solution is added when 55 ~ 80 DEG C, " starvation method " successively segmentation is adopted slowly to add BA and MMA, 70 DEG C of reaction 7 h, obtain nano-calcium carbonate polymer composite particle through aftertreatment.
embodiment 1: the present invention adopts method as follows: first use the MPTMS of nano-calcium carbonate 3.5% in toluene medium under ultrasonic disperse to its pre-treatment, suction filtration, dry, grinding.The SDS of metering, distilled water and through the nanometer C of surface preparation bright 3 is added in there-necked flask, pH to 8 ~ 9 are adjusted with ammoniacal liquor, heat up after ultrasonic disperse 5min, stir, KPS solution is added when 80 DEG C, " starvation method " successively segmentation is adopted slowly to add BA and MMA, 70 DEG C of reaction 7 h, obtain nano-calcium carbonate polymer composite particle through aftertreatment.
embodiment 2: the present invention adopts method as follows: first use the MPTMS of nano-calcium carbonate 3.5% in toluene medium under ultrasonic disperse to its pre-treatment, suction filtration, dry, grinding.The SDS of metering, distilled water and through the nanometer C of surface preparation bright 3 is added in there-necked flask, pH to 8 ~ 9 are adjusted with ammoniacal liquor, heat up after ultrasonic disperse 6min, stir, KPS solution is added when 75 DEG C, " starvation method " successively segmentation is adopted slowly to add BA and MMA, 70 DEG C of reaction 7 h, obtain nano-calcium carbonate polymer composite particle through aftertreatment.
embodiment 3: the present invention adopts method as follows: first use the MPTMS of nano-calcium carbonate 3.5% in toluene medium under ultrasonic disperse to its pre-treatment, suction filtration, dry, grinding.The SDS of metering, distilled water and through the nanometer C of surface preparation bright 3 is added in there-necked flask, pH to 8 ~ 9 are adjusted with ammoniacal liquor, heat up after ultrasonic disperse 7 min, stir, KPS solution is added when 70 DEG C, " starvation method " successively segmentation is adopted slowly to add BA and MMA, 70 DEG C of reaction 7 h, obtain nano-calcium carbonate polymer composite particle through aftertreatment.
embodiment 4: the present invention adopts method as follows: first use the MPTMS of nano-calcium carbonate 3.5% in toluene medium under ultrasonic disperse to its pre-treatment, suction filtration, dry, grinding.The SDS of metering, distilled water and through the nanometer C of surface preparation bright 3 is added in there-necked flask, pH to 8 ~ 9 are adjusted with ammoniacal liquor, heat up after ultrasonic disperse 6 min, stir, KPS solution is added when 65 DEG C, " starvation method " successively segmentation is adopted slowly to add BA and MMA, 70 DEG C of reaction 7 h, obtain nano-calcium carbonate polymer composite particle through aftertreatment.
Claims (5)
1. nano-calcium carbonate composite particles preparation method, is characterized in that: first use the MPTMS of nano-calcium carbonate 3.5% in toluene medium under ultrasonic disperse to its pre-treatment, suction filtration, dry, grinding; The SDS of metering, distilled water and through the nanometer C of surface preparation bright 3 is added in there-necked flask, pH to 8 ~ 9 are adjusted with ammoniacal liquor, heat up after ultrasonic disperse 5 ~ 10 min, stir, KPS solution is added when 55 ~ 80 DEG C, " starvation method " successively segmentation is adopted slowly to add BA and MMA, 70 DEG C of reaction 7 h, obtain nano-calcium carbonate polymer composite particle through aftertreatment.
2. nano-calcium carbonate composite particles preparation method according to claim 1, is characterized in that, first use the MPTMS of nano-calcium carbonate 3.5% in toluene medium under ultrasonic disperse to its pre-treatment, suction filtration, dry, grinding; The SDS of metering, distilled water and through the nanometer C of surface preparation bright 3 is added in there-necked flask, pH to 8 ~ 9 are adjusted with ammoniacal liquor, heat up after ultrasonic disperse 5min, stir, KPS solution is added when 80 DEG C, " starvation method " successively segmentation is adopted slowly to add BA and MMA, 70 DEG C of reaction 7 h, obtain nano-calcium carbonate polymer composite particle through aftertreatment.
3. nano-calcium carbonate composite particles preparation method according to claim 1, is characterized in that, first use the MPTMS of nano-calcium carbonate 3.5% in toluene medium under ultrasonic disperse to its pre-treatment, suction filtration, dry, grinding; The SDS of metering, distilled water and through the nanometer C of surface preparation bright 3 is added in there-necked flask, pH to 8 ~ 9 are adjusted with ammoniacal liquor, heat up after ultrasonic disperse 6min, stir, KPS solution is added when 75 DEG C, " starvation method " successively segmentation is adopted slowly to add BA and MMA, 70 DEG C of reaction 7 h, obtain nano-calcium carbonate polymer composite particle through aftertreatment.
4. nano-calcium carbonate composite particles preparation method according to claim 1, is characterized in that, first use the MPTMS of nano-calcium carbonate 3.5% in toluene medium under ultrasonic disperse to its pre-treatment, suction filtration, dry, grinding; The SDS of metering, distilled water and through the nanometer C of surface preparation bright 3 is added in there-necked flask, pH to 8 ~ 9 are adjusted with ammoniacal liquor, heat up after ultrasonic disperse 7 min, stir, KPS solution is added when 70 DEG C, " starvation method " successively segmentation is adopted slowly to add BA and MMA, 70 DEG C of reaction 7 h, obtain nano-calcium carbonate polymer composite particle through aftertreatment.
5. nano-calcium carbonate composite particles preparation method according to claim 1, is characterized in that, first use the MPTMS of nano-calcium carbonate 3.5% in toluene medium under ultrasonic disperse to its pre-treatment, suction filtration, dry, grinding; The SDS of metering, distilled water and through the nanometer C of surface preparation bright 3 is added in there-necked flask, pH to 8 ~ 9 are adjusted with ammoniacal liquor, heat up after ultrasonic disperse 6 min, stir, KPS solution is added when 65 DEG C, " starvation method " successively segmentation is adopted slowly to add BA and MMA, 70 DEG C of reaction 7 h, obtain nano-calcium carbonate polymer composite particle through aftertreatment.
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| CN201310417773.5A CN104448935A (en) | 2013-09-15 | 2013-09-15 | Preparation method for nano-calcium carbonate composite particle |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778569A (en) * | 2016-05-05 | 2016-07-20 | 中钛集团洛阳市裕星化工有限公司 | Method for preparing composite titanium dioxide powder with titanium-coated light calcium carbonate |
| CN106243779A (en) * | 2016-08-29 | 2016-12-21 | 潍坊大耀新材料有限公司 | A kind of process that inorganic powder material is carried out organic coating |
| CN106336690A (en) * | 2016-08-29 | 2017-01-18 | 潍坊大耀新材料有限公司 | Preparing technology of organic coating of high purity industrial product zinc sulfide powder |
-
2013
- 2013-09-15 CN CN201310417773.5A patent/CN104448935A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778569A (en) * | 2016-05-05 | 2016-07-20 | 中钛集团洛阳市裕星化工有限公司 | Method for preparing composite titanium dioxide powder with titanium-coated light calcium carbonate |
| CN105778569B (en) * | 2016-05-05 | 2017-10-31 | 中钛集团洛阳市裕星化工有限公司 | A kind of preparation method of the composite titanium dioxide of titanium cladding precipitated calcium carbonate |
| CN106243779A (en) * | 2016-08-29 | 2016-12-21 | 潍坊大耀新材料有限公司 | A kind of process that inorganic powder material is carried out organic coating |
| CN106336690A (en) * | 2016-08-29 | 2017-01-18 | 潍坊大耀新材料有限公司 | Preparing technology of organic coating of high purity industrial product zinc sulfide powder |
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Application publication date: 20150325 |
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