CN107022045A - latex microsphere and preparation method thereof - Google Patents
latex microsphere and preparation method thereof Download PDFInfo
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- CN107022045A CN107022045A CN201710296866.5A CN201710296866A CN107022045A CN 107022045 A CN107022045 A CN 107022045A CN 201710296866 A CN201710296866 A CN 201710296866A CN 107022045 A CN107022045 A CN 107022045A
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- phase solution
- latex microsphere
- latex
- carboxylated
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polymerisation Methods In General (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses a kind of latex microsphere, it is prepared from by following parts by weight of component：30 40 parts of styrene, 2.5 4 parts of acrylic acid, 8 12 parts of emulsifying agent, 0.2 0.4 parts of initiator, 1.5 2.5 parts of organic solvent, 10 20 parts of water.Latex microsphere size uniformity height, carboxylated completely, can effectively ensure that and the using effect after antibody coupling in the present invention.
Description
Technical field
The present invention relates to biomedicine field, more particularly to a kind of latex microsphere and preparation method thereof.
Background technology
Latex microsphere attracts increasing concern in the extensive use of biological, field of medicaments.In the prior art, latex is micro-
The size uniformity of ball is poor, and activated carboxylic rate is 80% or so thereon, during with antibody binding, and antibody distribution consistency degree is low, and
Skewness, limits sensitivity and causes antibody bioactive to reduce, mutability causes false negative；When by coupling agent with it is anti-
Body be coupled when, the amount of antibody being coated with thereon can be caused very high so that coated antibody surface steric hindrance increase and
The free degree is low, sensitivity and increase nonspecific reaction that the immune latex microsphere of reduction is determined.
The content of the invention
In order to overcome the deficiencies in the prior art, it is an object of the invention to provide size uniformity height, carboxylated are complete
Latex microsphere.
To solve the above problems, the technical solution adopted in the present invention is as follows：
A kind of latex microsphere, is prepared from by following parts by weight of component：
It is preferred that, it is prepared from by following parts by weight of component：
It is preferred that, the emulsifying agent is dodecyl sodium sulfate.
It is preferred that, the initiator is potassium peroxydisulfate or sodium peroxydisulfate.
It is preferred that, the organic solvent is hexadecane.
Present invention additionally comprises a kind of preparation method of latex microsphere, including：
S101. the preparation of aqueous phase solution：By emulsifying agent obtained aqueous phase solution soluble in water；
S102. the preparation of oil-phase solution：Oil-phase solution is constituted after styrene is mixed with organic solvent；
S103. the preparation of colostric fluid and first carboxylated：Aqueous phase solution, oil-phase solution are mixed to prepare under ultrasound condition
Colostric fluid, and by colostric fluid, initiator and 60%-70% acrylic acid add container for stirring it is uniform after, under nitrogen protection, 85
10h is reacted at DEG C；
S104. carboxylated again：Residual acrylic acid is added into the solution after reaction 12h, under nitrogen protection, 80 DEG C of reactions
6h, is produced.
Further, in addition to step S105. by emulsion breaking made from S104, centrifuge, collect product and use deionization
Water is cleaned, and gained is latex microsphere.
Further, ultrasound condition is that ultrasonic cell disruptor carries out ultrasound in 400W power in the step S103
Emulsification.
Compared with prior art, the beneficial effects of the present invention are：Latex microsphere size uniformity prepared by the present invention reaches
More than 98%, and realize the full carboxylated in present latex particulate surface and stably；The preparation method of present latex particulate is simple in the present invention, system
Standby cost of material is low, manufacturing cycle section, can be in large-scale application.
Brief description of the drawings
Fig. 1 is the preparation flow figure of present latex particulate in the present invention.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
The invention discloses a kind of latex microsphere, it is prepared from by following parts by weight of component：30-40 parts of styrene, propylene
It is sour 2.5-4 parts, 8-12 parts of emulsifying agent, 0.2-0.4 parts of initiator, 1.5-2.5 parts of organic solvent, 10-20 parts of water.
It is preferred that, it is prepared from by following parts by weight of component：36 parts of styrene, 4 parts of acrylic acid, 10 parts of emulsifying agent triggers
0.3 part of agent, 2 parts of organic solvent, 10 parts of water.
It is preferred that, the emulsifying agent is dodecyl sodium sulfate.The initiator is potassium peroxydisulfate or sodium peroxydisulfate.It is described
Organic solvent is hexadecane.
As shown in figure 1, present invention additionally comprises a kind of preparation method of latex microsphere, including：
S101. the preparation of aqueous phase solution：By emulsifying agent obtained aqueous phase solution soluble in water；
S102. the preparation of oil-phase solution：Oil-phase solution is constituted after styrene is mixed with organic solvent；
S103. the preparation of colostric fluid and first carboxylated：Aqueous phase solution, oil-phase solution are mixed to prepare under ultrasound condition
Colostric fluid, and by colostric fluid, initiator and 60%-70% acrylic acid add container for stirring it is uniform after, under nitrogen protection, 85
10h is reacted at DEG C；
S104. carboxylated again：Residual acrylic acid is added into the solution after reaction 12h, under nitrogen protection, 80 DEG C of reactions
6h, is produced.
Further, in addition to step S105. by emulsion breaking made from S104, centrifuge, collect product and use deionization
Water is cleaned, and gained is latex microsphere.
Further, ultrasound condition is that ultrasonic cell disruptor carries out ultrasound in 400W power in the step S103
Emulsification.
Embodiment 1
Flow prepares latex microsphere in reference picture 1
S101. the preparation of aqueous phase solution：8g dodecyl sodium sulfates are dissolved in 10g water aqueous phase solution is made；
S102. the preparation of oil-phase solution：Oil-phase solution is constituted after 30g styrene is mixed with 1.5g hexadecanes；
S103. the preparation of colostric fluid and first carboxylated：By aqueous phase solution, oil-phase solution in ultrasonic cell disruptor
400W power carries out ultrasonic emulsification and colostric fluid is made, and the acrylic acid of colostric fluid, 0.2g potassium peroxydisulfates and 1.8g is added into appearance
After being stirred in device, under nitrogen protection, 10h is reacted at 85 DEG C；
S104. carboxylated again：Residue 1.8g acrylic acid is added into the solution after reaction 12h, under nitrogen protection, 80 DEG C
6h is reacted, is produced.
S105. by emulsion breaking made from S104, centrifugation, collect product and cleaned with deionized water, gained is that latex is micro-
Ball.
After testing, the latex microsphere particle diameter of acquisition is between 55-65nm, and its size uniformity reaches more than 98%.Utilize
Conductimetric titration method detects that the full carboxylated in present latex particulate surface reaches more than 99.2%, and carboxylated is steady to carboxyl-content
Qualitative height, can effectively ensure that and the using effect after antibody coupling.
Embodiment 2
Flow prepares latex microsphere in reference picture 1
S101. the preparation of aqueous phase solution：10 dodecyl sodium sulfates are dissolved in 10g water aqueous phase solution is made；
S102. the preparation of oil-phase solution：Oil-phase solution is constituted after 36g styrene is mixed with 2g hexadecanes；
S103. the preparation of colostric fluid and first carboxylated：By aqueous phase solution, oil-phase solution in ultrasonic cell disruptor
400W power carries out ultrasonic emulsification and colostric fluid is made, and the acrylic acid of colostric fluid, 0.3g potassium peroxydisulfates and 2.4g is added into appearance
After being stirred in device, under nitrogen protection, 10h is reacted at 85 DEG C；
S104. carboxylated again：Residue 1.6g acrylic acid is added into the solution after reaction 12h, under nitrogen protection, 80 DEG C
6h is reacted, is produced.
S105. by emulsion breaking made from S104, centrifugation, collect product and cleaned with deionized water, gained is that latex is micro-
Ball.
After testing, the latex microsphere particle diameter of acquisition is between 55-65nm, and its size uniformity reaches more than 98.5%.Profit
Carboxyl-content is detected with conductance titration method, the full carboxylated in present latex particulate surface reaches more than 99.5%, and carboxylated
Stability is high, can effectively ensure that and the using effect after antibody coupling.
Embodiment 3
Flow prepares latex microsphere in reference picture 1
S101. the preparation of aqueous phase solution：12g dodecyl sodium sulfates are dissolved in 20g water aqueous phase solution is made；
S102. the preparation of oil-phase solution：Oil-phase solution is constituted after 40g styrene is mixed with 2.5g hexadecanes；
S103. the preparation of colostric fluid and first carboxylated：By aqueous phase solution, oil-phase solution in ultrasonic cell disruptor
400W power carries out ultrasonic emulsification and colostric fluid is made, and the acrylic acid of colostric fluid, 0.4g potassium peroxydisulfates and 2.8g is added into appearance
After being stirred in device, under nitrogen protection, 10h is reacted at 85 DEG C；
S104. carboxylated again：Residue 1.2g acrylic acid is added into the solution after reaction 12h, under nitrogen protection, 80 DEG C
6h is reacted, is produced.
S105. by emulsion breaking made from S104, centrifugation, collect product and cleaned with deionized water, gained is that latex is micro-
Ball.
After testing, the latex microsphere particle diameter of acquisition is between 55-65nm, and its size uniformity reaches more than 98.1%.Profit
Carboxyl-content is detected with conductance titration method, the full carboxylated in present latex particulate surface reaches more than 99.1%, and carboxylated
Stability is high, can effectively ensure that and the using effect after antibody coupling.
Embodiment 4
Flow prepares latex microsphere in reference picture 1
S101. the preparation of aqueous phase solution：10g dodecyl sodium sulfates are dissolved in 15g water aqueous phase solution is made；
S102. the preparation of oil-phase solution：Oil-phase solution is constituted after 36g styrene is mixed with 2.5g hexadecanes；
S103. the preparation of colostric fluid and first carboxylated：By aqueous phase solution, oil-phase solution in ultrasonic cell disruptor
400W power carries out ultrasonic emulsification and colostric fluid is made, and the acrylic acid of colostric fluid, 0.4g potassium peroxydisulfates and 2.8g is added into appearance
After being stirred in device, under nitrogen protection, 10h is reacted at 85 DEG C；
S104. carboxylated again：Residue 1.2g acrylic acid is added into the solution after reaction 12h, under nitrogen protection, 80 DEG C
6h is reacted, is produced.
S105. by emulsion breaking made from S104, centrifugation, collect product and cleaned with deionized water, gained is that latex is micro-
Ball.
After testing, the latex microsphere particle diameter of acquisition is between 55-65nm, and its size uniformity reaches more than 98.2%.Profit
Carboxyl-content is detected with conductance titration method, the full carboxylated in present latex particulate surface reaches more than 99.3%, and carboxylated
Stability is high, can effectively ensure that and the using effect after antibody coupling.
It will be apparent to those skilled in the art that technical scheme that can be as described above and design, make other various
It is corresponding to change and deformation, and all these change and deformation should all belong to the protection domain of the claims in the present invention
Within.
Claims (8)
1. a kind of latex microsphere, it is characterised in that be prepared from by following parts by weight of component：
2. latex microsphere as claimed in claim 1, it is characterised in that be prepared from by following parts by weight of component：
3. latex microsphere as claimed in claim 1, it is characterised in that the emulsifying agent is dodecyl sodium sulfate.
4. latex microsphere as claimed in claim 1, it is characterised in that the initiator is potassium peroxydisulfate or sodium peroxydisulfate.
5. latex microsphere as claimed in claim 1, it is characterised in that the organic solvent is hexadecane.
6. the preparation method of any one of the claim 1-5 latex microspheres, including：
S101. the preparation of aqueous phase solution：By emulsifying agent obtained aqueous phase solution soluble in water；
S102. the preparation of oil-phase solution：Oil-phase solution is constituted after styrene is mixed with organic solvent；
S103. the preparation of colostric fluid and first carboxylated：Aqueous phase solution, oil-phase solution are mixed to prepare colostrum under ultrasound condition
Liquid, and by colostric fluid, initiator and 60%-70% acrylic acid add container for stirring it is uniform after, under nitrogen protection, at 85 DEG C
React 10h；
S104. carboxylated again：Residual acrylic acid is added into the solution after reaction 12h, under nitrogen protection, 80 DEG C of reaction 6h,
Produce.
7. the preparation method of latex microsphere as claimed in claim 6, it is characterised in that also including step S105. by S104 systems
Emulsion breaking, centrifugation, collection product and cleaned with deionized water, gained is latex microsphere.
8. the preparation method of latex microsphere as claimed in claim 6, it is characterised in that ultrasound condition is in the step S103
Ultrasonic cell disruptor carries out ultrasonic emulsification in 400W power.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710296866.5A CN107022045B (en) | 2017-04-28 | 2017-04-28 | Latex microsphere and preparation method thereof |
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|---|---|---|---|
| CN201710296866.5A CN107022045B (en) | 2017-04-28 | 2017-04-28 | Latex microsphere and preparation method thereof |
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| Publication Number | Publication Date |
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| CN107022045A true CN107022045A (en) | 2017-08-08 |
| CN107022045B CN107022045B (en) | 2019-07-02 |
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| CN201710296866.5A Active CN107022045B (en) | 2017-04-28 | 2017-04-28 | Latex microsphere and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111607103A (en) * | 2020-06-30 | 2020-09-01 | 福隆医疗器械集团有限公司 | Alkyl phosphono modified collagen-based material, preparation method, modified collagen and application |
| CN111892736A (en) * | 2020-08-13 | 2020-11-06 | 上海科华生物工程股份有限公司 | Polystyrene microsphere for improving sensitivity of latex turbidimetry and preparation method thereof |
Citations (3)
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| CN102492075A (en) * | 2011-12-08 | 2012-06-13 | 天津医科大学 | Nanometer carboxylated polystyrene microsphere with spacer arm and preparation method thereof |
| CN104311715A (en) * | 2014-10-25 | 2015-01-28 | 陕西玉航电子有限公司 | Preparation method of colloidal microspheres |
| CN104558351A (en) * | 2013-10-21 | 2015-04-29 | 大连市沙河口区中小微企业服务中心 | Method of surface carboxyl modification of nano/submicron particles |
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2017
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Patent Citations (3)
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| CN102492075A (en) * | 2011-12-08 | 2012-06-13 | 天津医科大学 | Nanometer carboxylated polystyrene microsphere with spacer arm and preparation method thereof |
| CN104558351A (en) * | 2013-10-21 | 2015-04-29 | 大连市沙河口区中小微企业服务中心 | Method of surface carboxyl modification of nano/submicron particles |
| CN104311715A (en) * | 2014-10-25 | 2015-01-28 | 陕西玉航电子有限公司 | Preparation method of colloidal microspheres |
Non-Patent Citations (1)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111607103A (en) * | 2020-06-30 | 2020-09-01 | 福隆医疗器械集团有限公司 | Alkyl phosphono modified collagen-based material, preparation method, modified collagen and application |
| CN111607103B (en) * | 2020-06-30 | 2022-05-17 | 江苏创健医疗科技有限公司 | Alkyl phosphono modified collagen-based material, preparation method, modified collagen and application |
| CN111892736A (en) * | 2020-08-13 | 2020-11-06 | 上海科华生物工程股份有限公司 | Polystyrene microsphere for improving sensitivity of latex turbidimetry and preparation method thereof |
| CN111892736B (en) * | 2020-08-13 | 2022-08-26 | 上海科华生物工程股份有限公司 | Polystyrene microsphere for improving sensitivity of latex turbidimetry and preparation method thereof |
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| CN107022045B (en) | 2019-07-02 |
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Address after: 213000 No. 18 Jincheng Road, Wujin Economic Development Zone, Changzhou City, Jiangsu Province Applicant after: Fulong Medical Devices Group Co., Ltd. Address before: 213000 No. 18 Jincheng Road, Wujin Economic Development Zone, Changzhou City, Jiangsu Province Applicant before: Fulong medical materials Co. Ltd. (China) |
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