CN107199002A - A kind of preparation method of cationic perfume microcapsules - Google Patents
A kind of preparation method of cationic perfume microcapsules Download PDFInfo
- Publication number
- CN107199002A CN107199002A CN201710338975.9A CN201710338975A CN107199002A CN 107199002 A CN107199002 A CN 107199002A CN 201710338975 A CN201710338975 A CN 201710338975A CN 107199002 A CN107199002 A CN 107199002A
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- preparation
- mixed
- cationic
- microcapsules
- perfume microcapsules
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/005—Compositions containing perfumes; Compositions containing deodorants
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Fats And Perfumes (AREA)
- Cosmetics (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The present invention relates to microcapsules field, more particularly to a kind of preparation method of cationic perfume microcapsules.According to the preparation of raw material, emulsification shearing, regulation pH, preliminary wall building, secondary wall building and prepare the processing step of final product and prepare cationic perfume microcapsules.Perfume microcapsule prepared by the present invention carries cationic, can be more firm and difficult for drop-off in combination with the fabric of anionic property, greatly reduces the loss of microcapsules on cloth, improves the fragrance retention and utilization rate of perfume microcapsule.The preparation method of invention is simple and easy to apply, inexpensive, and aftertreatment technology is simple, is conducive to the propulsion of batch production.
Description
Technical field
The present invention relates to microcapsules field, more particularly to a kind of preparation method of cationic perfume microcapsules.
Background technology
Microcapsules are the spherical minute bubbles that a class has certain permeability, and outer layer is pellicle, and inside is aqueous kernel.Will
After micro-encapsulation of core material, it is completely cut off with external environment, from the influence of the factors such as ambient temperature, humidity, oxygen, improve core
Again its property can be kept to be basically unchanged while stability, and under certain condition, such as rub, collide outside stimulus, make wall
Material is destroyed, and core is released slowly, and reaches the purpose of sustained release and controlled release.Since A.M.Sun inventions sodium alginate/poly- relies
Since propylhomoserin microcapsules, microcapsules technology is widely used in microorganism, animal and plant cells, enzyme and bioactive substance and chemistry
The fields such as the immobilization of medicine.Perfume microcapsule is a branch in microcapsules technology, is that a kind of core is essence or spices
Microcapsules, at present in medicine, food, weaving, construction material, agricultural chemicals, coating, ink, adhesive, cosmetics, detergent etc.
Industry achieves wide application.
Traditional perfume microcapsule in dyeing and finishing fabric because spices tack does not cause its easy to fall off by force, fragrance remaining time
It is short；Microcapsules prepared by the padding method used in the dyeing and finishing fabric residual quantity in water is high, and utilization rate is low.
The content of the invention
The technical problem to be solved in the present invention is：In order to solve fragrance remaining time during traditional perfume microcapsule dyeing and finishing fabric it is short,
The problem of utilization rate is low, the present invention provides a kind of preparation method of cationic perfume microcapsules.
The technical solution adopted for the present invention to solve the technical problems is：A kind of preparation side of cationic perfume microcapsules
Method, concrete operation step includes：
(1) preparation of raw material, is in mass ratio 1：4-6：8-12 ratio weighs fragrance essential oil, fabric finishing agent and water,
It is well mixed, form mixed solution；
(2) emulsification shearing, the mixing for weighing above-mentioned fragrance essential oil quality 6-10% crosslinking agent addition step (1) preparation is molten
In liquid, 20-30min is sheared with 10000r/min shear rate with high-shear emulsion machine, homogeneous phase solution is formed；
(3) pH is adjusted, glacial acetic acid is added dropwise in homogeneous phase solution prepared by step (2) and analyzes pure regulation pH to 4-5, acid is formed
Property homogeneous phase solution；
(4) preliminary wall building, weighs above-mentioned fragrance essential oil quality 30-50% resin prepolymer, according to resin prepolymer with
Water quality ratio is 1：3-5 ratio weighs corresponding water, and the acidity prepared into step (3) is added dropwise after both are sufficiently mixed dropwise
In homogeneous phase solution, control rate of addition is in every drop 20-40s, using 30 DEG C of heating water baths, while controlling mixing speed in 400-
500r/min then by heating water bath is to 55 DEG C and is incubated 1-1.5h, forms mixed material until completion of dropping；
(5) secondary wall building and final product is prepared, mixed material prepared by step (4) is cooled to after room temperature, is weighed
Above-mentioned fragrance essential oil quality 30-50% resin prepolymer, is 1 according to resin prepolymer and water quality ratio：3-5 ratio is weighed
Corresponding water, is added dropwise in the mixed material prepared into step (4) dropwise after both are sufficiently mixed, and control rate of addition is in every drop
20-40s, using 30 DEG C of heating water baths, while controlling mixing speed in 400-500r/min up to completion of dropping, then by water-bath
It is heated to 55 DEG C and is incubated 2-2.5h, be again heated to after 65 DEG C and be incubated 1-1.5h, weak aqua ammonia is added dropwise after cooling and analyzes pure regulation
Cationic perfume microcapsules are made to 7-8 in pH.
Preferably, step (1) the fabric finishing agent is 1-METHYLPYRROLIDONE disulfate.
Preferably, the crosslinking agent described in step (2) is A-9 crosslinking agents.
Preferably, the resin prepolymer described in step (4) is base polyurethane prepolymer for use as；Resin prepolymer described in step (5)
Body is base polyurethane prepolymer for use as.
The beneficial effects of the invention are as follows fabric finishing agent of the invention is cationic dyeing and finishing agent and serves as emulsifying agent, is had
There is extremely strong surface-active and the oil-water interfacial film of densification can be formed, play what is promoted and protect in the forming process of microcapsules
Effect, while allowing perfume microcapsule to produce cationic.Perfume microcapsule prepared by the present invention carry cationic, can with the moon from
The fabric of sub- property is more firm and difficult for drop-off in combination, greatly reduces the loss of microcapsules on cloth, improves spices micro-
The fragrance retention and utilization rate of capsule.The preparation method of invention is simple and easy to apply, inexpensive, and aftertreatment technology is simple, is conducive to
The propulsion of batch production.
Embodiment
The present invention is described in more detail below by reference to embodiment, but protection scope of the present invention is not limited
In these embodiments.
Embodiment 1
(1) preparation of raw material, weighs fabric finishing agent and the 80g water of 10g fragrance essential oil, 40g, is well mixed, shape
Into mixed solution；
(2) emulsification shearing, the A-9 crosslinking agents for weighing 0.6g are added in mixed solution prepared by step (1), with high shear breast
Change machine shears 25min with 10000r/min shear rate, forms homogeneous phase solution；
(3) pH is adjusted, glacial acetic acid is added dropwise in homogeneous phase solution prepared by step (2) and analyzes pure regulation pH to 4-5, acid is formed
Property homogeneous phase solution；
(4) preliminary wall building, weighs 3g base polyurethane prepolymer for use as and 9g water, is added dropwise dropwise after being sufficiently mixed into step (3)
In the acid homogeneous phase solution of preparation, control rate of addition is in every drop 25-35s, using 30 DEG C of heating water baths, while controlling stirring speed
Degree until completion of dropping, then by heating water bath is to 55 DEG C and is incubated 1h, forms mixed material in 450r/min；
(5) secondary wall building and final product is prepared, when the mixed material of step (4) is cooled into room temperature, weighs the poly- of 3g
The water of urethane performed polymer and 9g, is added dropwise in the mixed material prepared into step (4) dropwise after being sufficiently mixed, and control rate of addition exists
25-35s is often dripped, using 30 DEG C of heating water baths, while controlling mixing speed in 450r/min up to completion of dropping, then by water-bath
It is heated to 55 DEG C and is incubated 2h, 1h is incubated after being again heated to 65 DEG C；Weak aqua ammonia is added dropwise after cooling and analyzes pure regulation pH to 7-8,
Cationic perfume microcapsules are made.
Embodiment 2
(1) preparation of raw material, weighs fabric finishing agent and the 100g water of 10g fragrance essential oil, 50g, is well mixed, shape
Into mixed solution；
(2) emulsification shearing, the A-9 crosslinking agents for weighing 0.8g are added in mixed solution prepared by step (1), with high shear breast
Change machine shears 25min with 10000r/min shear rate, forms homogeneous phase solution；
(3) pH is adjusted, glacial acetic acid is added dropwise in homogeneous phase solution prepared by step (2) and analyzes pure regulation pH to 4-5, acid is formed
Property homogeneous phase solution；
(4) preliminary wall building, weighs 4g base polyurethane prepolymer for use as and 16g water, is added dropwise dropwise after being sufficiently mixed into step (3)
In the acid homogeneous phase solution of preparation, control rate of addition is in every drop 25-35s, using 30 DEG C of heating water baths, while controlling stirring speed
Degree until completion of dropping, then by heating water bath is to 55 DEG C and is incubated 1.5h, forms mixed material in 450r/min；
(5) secondary wall building and final product is prepared, when the mixed material of step (4) is cooled into room temperature, weighs the poly- of 4g
The water of urethane performed polymer and 16g, is added dropwise in the mixed material prepared into step (4) dropwise after being sufficiently mixed, and controls rate of addition
In every drop 25-35s, using 30 DEG C of heating water baths, while controlling mixing speed in 450r/min up to completion of dropping, then by water
Bath is heated to 55 DEG C and is incubated 2h, and 1h is incubated after being again heated to 65 DEG C；Weak aqua ammonia is added dropwise after cooling and analyzes pure regulation pH to 7-
8, cationic perfume microcapsules are made.
Embodiment 3
(1) preparation of raw material, weighs fabric finishing agent and the 120g water of 10g fragrance essential oil, 60g, is well mixed, shape
Into mixed solution；
(2) emulsification shearing, the A-9 crosslinking agents for weighing 1g are added in mixed solution prepared by step (1), use high-shear emulsifying
Machine shears 25min with 10000r/min shear rate, forms homogeneous phase solution；
(3) pH is adjusted, glacial acetic acid is added dropwise in homogeneous phase solution prepared by step (2) and analyzes pure regulation pH to 4-5, acid is formed
Property homogeneous phase solution；
(4) preliminary wall building, weighs 5g base polyurethane prepolymer for use as and 20g water, is added dropwise dropwise after being sufficiently mixed into step (3)
In the acid homogeneous phase solution of preparation, control rate of addition is in every drop 25-35s, using 30 DEG C of heating water baths, while controlling stirring speed
Degree until completion of dropping, then by heating water bath is to 55 DEG C and is incubated 1.5h, forms mixed material in 450r/min；
(5) secondary wall building and final product is prepared, when the mixed material of step (4) is cooled into room temperature, weighs the poly- of 5g
The water of urethane performed polymer and 20g, is added dropwise in the mixed material prepared into step (4) dropwise after being sufficiently mixed, and controls rate of addition
In every drop 25-35s, using 30 DEG C of heating water baths, while controlling mixing speed in 450r/min up to completion of dropping, then by water
Bath is heated to 55 DEG C and is incubated 2h, and 1h is incubated after being again heated to 65 DEG C；Weak aqua ammonia is added dropwise after cooling and analyzes pure regulation pH to 7-
8, cationic perfume microcapsules are made.
Using the above-mentioned desirable embodiment according to the present invention as enlightenment, by above-mentioned description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to its technical scope is determined according to right.
Claims (4)
1. a kind of preparation method of cationic perfume microcapsules, it is characterised in that the concrete operation step bag of the preparation method
Include：
(1) it is 1 in mass ratio：4-6：8-12 ratio weighs fragrance essential oil, fabric finishing agent and water, is well mixed, and forms mixed
Close solution；
(2) crosslinking agent for weighing above-mentioned fragrance essential oil quality 6-10% is added in mixed solution prepared by step (1), uses high shear
Mulser shears 20-30min with 10000r/min shear rate, forms homogeneous phase solution；
(3) glacial acetic acid is added dropwise in homogeneous phase solution prepared by step (2) and analyzes pure regulation pH to 4-5, form acid homogeneous phase solution；
(4) above-mentioned fragrance essential oil quality 30-50% wall material 1 is weighed, is 1 according to wall material 1 and water quality ratio：3-5 ratio claims
Corresponding water is taken, is added dropwise dropwise after both are sufficiently mixed in the acid homogeneous phase solution prepared into step (3), rate of addition is controlled
In every drop 20-40s, using 30 DEG C of heating water baths, while controlling mixing speed in 400-500r/min until completion of dropping, then
By heating water bath is to 55 DEG C and is incubated 1-1.5h, mixed material is formed；
(5) mixed material of step (4) is cooled to after room temperature, weighs above-mentioned fragrance essential oil quality 30-50% wall material 2, press
Screen wall facing the gate of a house material 1 is 1 with water quality ratio：3-5 ratio weighs corresponding water, is added dropwise dropwise after both are sufficiently mixed into step (4)
In the mixed material of preparation, control rate of addition is in every drop 20-40s, using 30 DEG C of heating water baths, while controlling mixing speed to exist
400-500r/min then by heating water bath is to 55 DEG C and is incubated 2-2.5h, is again heated to after 65 DEG C and is incubated until completion of dropping
1-1.5h；Weak aqua ammonia is added dropwise after cooling and analyzes pure regulation pH to 7-8, cationic perfume microcapsules are made.
2. the preparation method of cationic perfume microcapsules as claimed in claim 1, it is characterised in that step (1) described fabric
Dyeing and finishing agent is 1-METHYLPYRROLIDONE disulfate.
3. the preparation method of cationic perfume microcapsules as claimed in claim 1, it is characterised in that the friendship described in step (2)
Connection agent is A-9 crosslinking agents.
4. the preparation method of cationic perfume microcapsules as claimed in claim 1, it is characterised in that the tree described in step (4)
Fat performed polymer is base polyurethane prepolymer for use as；Resin prepolymer described in step (5) is base polyurethane prepolymer for use as.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710338975.9A CN107199002B (en) | 2017-05-15 | 2017-05-15 | Preparation method of cationic perfume microcapsule |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710338975.9A CN107199002B (en) | 2017-05-15 | 2017-05-15 | Preparation method of cationic perfume microcapsule |
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| Publication Number | Publication Date |
|---|---|
| CN107199002A true CN107199002A (en) | 2017-09-26 |
| CN107199002B CN107199002B (en) | 2020-04-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710338975.9A Active CN107199002B (en) | 2017-05-15 | 2017-05-15 | Preparation method of cationic perfume microcapsule |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117162597A (en) * | 2023-10-12 | 2023-12-05 | 广州三森健康产业科技有限公司 | Breathable and antibacterial self-heating combined material and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090186058A1 (en) * | 2004-09-14 | 2009-07-23 | Ronald Lee Hart | Microencapsulation of biocides and antifouling agents |
| CN103642591A (en) * | 2013-06-30 | 2014-03-19 | 金玛瑙香水（明光）有限公司 | Microcapsule spice composition |
| CN104975513A (en) * | 2015-05-29 | 2015-10-14 | 天津城建大学 | Efficient antibacterial chitosan essential oil microcapsule preparation method |
| CN105921085A (en) * | 2016-05-10 | 2016-09-07 | 天津市双马香精香料新技术有限公司 | Preparation method of compound emulsifier in-situ crosslinking chitosan quaternary ammonium salt essential oil microcapsule |
-
2017
- 2017-05-15 CN CN201710338975.9A patent/CN107199002B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090186058A1 (en) * | 2004-09-14 | 2009-07-23 | Ronald Lee Hart | Microencapsulation of biocides and antifouling agents |
| CN103642591A (en) * | 2013-06-30 | 2014-03-19 | 金玛瑙香水（明光）有限公司 | Microcapsule spice composition |
| CN104975513A (en) * | 2015-05-29 | 2015-10-14 | 天津城建大学 | Efficient antibacterial chitosan essential oil microcapsule preparation method |
| CN105921085A (en) * | 2016-05-10 | 2016-09-07 | 天津市双马香精香料新技术有限公司 | Preparation method of compound emulsifier in-situ crosslinking chitosan quaternary ammonium salt essential oil microcapsule |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117162597A (en) * | 2023-10-12 | 2023-12-05 | 广州三森健康产业科技有限公司 | Breathable and antibacterial self-heating combined material and preparation method and application thereof |
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| Publication number | Publication date |
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| CN107199002B (en) | 2020-04-28 |
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Effective date of registration: 20211223 Address after: 213016 third floor, building 7, No. 8, Lanxiang Road, West Taihu science and Technology Industrial Park, Changzhou City, Jiangsu Province Patentee after: CHANGZHOU MYSUN BIOLOGICAL MATERIALS CO.,LTD. Address before: Gehu Lake Road Wujin District 213164 Jiangsu city of Changzhou province No. 1 Patentee before: CHANGZHOU University |
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