CN100396842C - Method for preparing polyurethane fragrant microcapsules - Google Patents
Method for preparing polyurethane fragrant microcapsules Download PDFInfo
- Publication number
- CN100396842C CN100396842C CNB2006100960389A CN200610096038A CN100396842C CN 100396842 C CN100396842 C CN 100396842C CN B2006100960389 A CNB2006100960389 A CN B2006100960389A CN 200610096038 A CN200610096038 A CN 200610096038A CN 100396842 C CN100396842 C CN 100396842C
- Authority
- CN
- China
- Prior art keywords
- preparation
- polyethylene glycol
- oil phase
- cyclohexane
- fragrant microcapsules
- 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.)
- Expired - Fee Related
Links
- 239000003094 microcapsule Substances 0.000 title claims abstract description 18
- 239000004814 polyurethane Substances 0.000 title claims abstract description 13
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 13
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 13
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 239000005056 polyisocyanate Substances 0.000 claims abstract description 9
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims description 19
- 239000012071 phase Substances 0.000 claims description 12
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 10
- 235000010413 sodium alginate Nutrition 0.000 claims description 10
- 229940005550 sodium alginate Drugs 0.000 claims description 10
- 239000000661 sodium alginate Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000008346 aqueous phase Substances 0.000 claims description 5
- 239000000839 emulsion Substances 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 2
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000003754 machining Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- SFDZETWZUCDYMD-UHFFFAOYSA-N monosodium acetylide Chemical compound [Na+].[C-]#C SFDZETWZUCDYMD-UHFFFAOYSA-N 0.000 abstract 1
- 239000003205 fragrance Substances 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 235000013599 spices Nutrition 0.000 description 5
- 239000002775 capsule Substances 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 206010011732 Cyst Diseases 0.000 description 1
- 235000018958 Gardenia augusta Nutrition 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 244000178870 Lavandula angustifolia Species 0.000 description 1
- 235000010663 Lavandula angustifolia Nutrition 0.000 description 1
- 244000246386 Mentha pulegium Species 0.000 description 1
- 235000016257 Mentha pulegium Nutrition 0.000 description 1
- 235000004357 Mentha x piperita Nutrition 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 208000031513 cyst Diseases 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 235000001050 hortel pimenta Nutrition 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000001102 lavandula vera Substances 0.000 description 1
- 235000018219 lavender Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Landscapes
- Fats And Perfumes (AREA)
Abstract
The invention relates to a manufacture method for polyurethane aroma microcapsule that is made up of polyisocyanate, essence and cyclohexane. Water phase is made up of sodium hydroxide, sodium acetylide, and deionized water. It includes the following steps: adding polyethylene glycol and acetone into oil phase, dropping into water phase for 1.5-2 hours, whisking at 400-600 rounds per minutes, keeping temperature at 40-60 degree centigrade, heating to 50-70 degree centigrade, taking reaction for 1-1.5 hour, filtering the product. The diameter of microcapsule is 20-4um, and it has high slow releasing ability. The machining of the microcapsule is convenient.
Description
Technical field
The present invention relates to a kind of weaving aromatic micro-capsule, especially relate to a kind of preparation of polyurethane fragrant microcapsules.
Background technology
Aromatic micro-capsule is by spices and be wrapped in outer capsule material and constitute, and particle diameter is at 20-40um.Aromatic micro-capsule is widely used in textile industry, and main effect has: reduce spices and extraneous contacting, thereby prevent that the spices volatilization is too fast, reduce fragrance loss, have certain slow releasing function, and prolong fragrance remaining time.Its capsule material of aromatic micro-capsule in the past adopts melamino-formaldehyde resinoid, materials such as gelatin mostly.Since problems such as there is the cyst wall instability in it, and porosity is irregular, so its slow release is not high, short with the spices fragrance remaining time of its parcel, and these materials adopt the preparation of oiliness system, some monomer free sometimes mostly.Do not meet environmental requirement.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, provide a kind of fragrance slow release higher, the preparation method of the preparation of environment amenable polyurethane fragrant microcapsules.
The object of the present invention is achieved like this: a kind of preparation method of polyurethane fragrant microcapsules is characterized in that: the oil phase of the preparation material of polyurethane fragrant microcapsules is made up of polyisocyanates, essence and cyclohexane; Water is made up of NaOH, sodium alginate, deionized water; Preparation technology adds polyethylene glycol and acetone in above-mentioned oil phase, be added dropwise to aqueous phase after the mixing, 1.5-2 hour drip off, mixing speed is at 400-600 rev/min, temperature remains on 40-60 ℃, after dripping off, be warming up to 50-70 ℃, reacted 1-1.5 hour, the product suction filtration that obtains, product is a white emulsion, and the proportioning of the each component of its preparation material is:
Oil phase:
Polyisocyanates 3.33-4.12g
Essence 19g
Cyclohexane 20～25ml
Water:
15% NaOH 2ml
Sodium alginate 0.3g
Deionized water 200ml;
Polyethylene glycol 3.0g;
Acetone 40～60ml.
Polyisocyanates of the present invention can be IPDI, TDI or HDI.
Molecular weight polyethylene glycol of the present invention can be 400,600 or 800.
Because polyisocyanates belongs to an indispensable monomer of polyurethane, can give the polyurethane resilience, high-modulus, the present invention uses polyisocyanates that spices is coated, the aromatic micro-capsule fragrance slow release that obtains is higher, environmentally friendly, environmental protection more, and the capsule material has certain resilience, is easy to processing.
The specific embodiment
Preparation method of the present invention is as follows:
Embodiment 1:
One, gets the raw materials ready
Oil phase: IPDI3.33g, cream jasmin france 19g, cyclohexane: 25ml.
Water: NaOH (15%) 2ml, deionized water 200ml, sodium alginate 0.3g.
The polyethylene glycol 3.0g of molecular weight 600.
Two, preparation technology
A, by said ratio, with the 200ml deionized water under high-speed stirred, dissolving 0.3g sodium alginate,
B, oil phase, polyethylene glycol are mixed with 40ml acetone,, under 500 rev/mins of conditions of mixing speed, are added drop-wise to aqueous phase, dripped off in 2 hours at 50 ℃,
C, be warming up to 60 ℃, continue reaction 1.5 hours,
D, crude product is carried out suction filtration, washing,
E, vacuumize, remove acetone and cyclohexane, product is a white emulsion.
Embodiment 2:
One, gets the raw materials ready
Oil phase: HDI:4.12g, peppermint essence 19g, cyclohexane 25ml.
Water: NaOH (15%) 2ml, deionized water: 200ml, sodium alginate: 0.3g.
The polyethylene glycol 3.0g of molecular weight 400.
Two, preparation method
A, by said ratio, with the 200ml deionized water under high-speed stirred, dissolving 0.3g sodium alginate,
B, oil phase, polyethylene glycol are mixed with 50ml acetone,, under 600 rev/mins of conditions of mixing speed, are added drop-wise to aqueous phase, dripped off in 1.5 hours at 50 ℃,
C, be warming up to 60 ℃, continue reaction 1 hour,
D, crude product is carried out suction filtration, washing,
E, vacuumize, remove acetone and cyclohexane, product is a white emulsion.
Embodiment 3:
One, gets the raw materials ready
Oil phase: TDI3.90g, lavender fragrance 19g carries zinc silica 2g, cyclohexane 25ml.
Water: NaOH (15%) 2ml, deionized water: 200ml, sodium alginate: 0.3g.
The polyethylene glycol 3.0g of molecular weight 800.
Two, preparation method
A, by said ratio, with the 200ml deionized water under high-speed stirred, dissolving 0.3g sodium alginate,
B, oil phase, polyethylene glycol are mixed with 60ml acetone,, under 600 rev/mins of conditions of mixing speed, are added drop-wise to aqueous phase, dripped off in 1.5 hours at 60 ℃,
C, be warming up to 70 ℃, continue reaction 1 hour,
D, crude product is carried out suction filtration, washing,
E, vacuumize, remove acetone and cyclohexane, product is a white emulsion.
Claims (3)
1. the preparation method of a polyurethane fragrant microcapsules, it is characterized in that: the oil phase of the preparation material of polyurethane fragrant microcapsules is made up of polyisocyanates, essence and cyclohexane; Water is made up of NaOH, sodium alginate, deionized water; Preparation technology adds polyethylene glycol and acetone in above-mentioned oil phase, be added dropwise to aqueous phase after the mixing, 1.5-2 hour drip off, mixing speed is at 400-600 rev/min, temperature remains on 40-60 ℃, after dripping off, be warming up to 50-70 ℃, reacted 1-1.5 hour, the product suction filtration that obtains, product is a white emulsion, and the proportioning of the each component of its preparation material is:
Oil phase:
Polyisocyanates 3.33-4.12g
Essence 19g
Cyclohexane 20～25ml;
Water:
15% NaOH 2ml
Sodium alginate 0.3g
Deionized water 200ml;
Polyethylene glycol 3.0g;
Acetone 40～60ml.
2. the preparation method of a kind of polyurethane fragrant microcapsules according to claim 1, it is characterized in that: described polyisocyanates is IPDI, TDI or HDI.
3. the preparation method of a kind of polyurethane fragrant microcapsules according to claim 1 and 2, it is characterized in that: described molecular weight polyethylene glycol is 400,600 or 800.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100960389A CN100396842C (en) | 2006-09-14 | 2006-09-14 | Method for preparing polyurethane fragrant microcapsules |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100960389A CN100396842C (en) | 2006-09-14 | 2006-09-14 | Method for preparing polyurethane fragrant microcapsules |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1936170A CN1936170A (en) | 2007-03-28 |
| CN100396842C true CN100396842C (en) | 2008-06-25 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100960389A Expired - Fee Related CN100396842C (en) | 2006-09-14 | 2006-09-14 | Method for preparing polyurethane fragrant microcapsules |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100396842C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101368219B (en) * | 2008-10-07 | 2012-09-26 | 四川大学 | Fragrant sustained-release type leather compound tanning agent and method of producing the same |
| CN102493182A (en) * | 2011-12-06 | 2012-06-13 | 东华大学 | Preparation method of Lyocell fabric with fatigue removing function |
| CN103194911B (en) * | 2013-04-27 | 2014-10-01 | 上海洋帆实业有限公司 | Mosquito-repellent fabric and preparation method thereof |
| CN111534901B (en) * | 2020-05-20 | 2022-02-22 | 杭州旺尚家纺有限公司 | Mosquito-proof insect-repellent and aromatic curtain fabric and preparation method thereof |
| CN113180292A (en) * | 2021-04-30 | 2021-07-30 | 深圳波顿香料有限公司 | Slow-release blasting bead and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5615836A (en) * | 1979-07-19 | 1981-02-16 | Mitsubishi Paper Mills Ltd | Micro capsule |
| CN1034103C (en) * | 1990-06-25 | 1997-02-26 | 高韵苕 | Encapsulate method of an essence micro-capsule |
| CN1429657A (en) * | 2001-12-31 | 2003-07-16 | 高韵苕 | Method of forming essence microcapsule using interface polymerization reaction |
| CN1501837A (en) * | 2001-04-10 | 2004-06-02 | 拜尔农作物科学股份公司 | Microcapsules |
| CN1805784A (en) * | 2003-05-11 | 2006-07-19 | 内盖夫研发局属本古里昂大学 | Encapsulated essential oils |
-
2006
- 2006-09-14 CN CNB2006100960389A patent/CN100396842C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5615836A (en) * | 1979-07-19 | 1981-02-16 | Mitsubishi Paper Mills Ltd | Micro capsule |
| CN1034103C (en) * | 1990-06-25 | 1997-02-26 | 高韵苕 | Encapsulate method of an essence micro-capsule |
| CN1501837A (en) * | 2001-04-10 | 2004-06-02 | 拜尔农作物科学股份公司 | Microcapsules |
| CN1429657A (en) * | 2001-12-31 | 2003-07-16 | 高韵苕 | Method of forming essence microcapsule using interface polymerization reaction |
| CN1805784A (en) * | 2003-05-11 | 2006-07-19 | 内盖夫研发局属本古里昂大学 | Encapsulated essential oils |
Non-Patent Citations (2)
| Title |
|---|
| 聚氨酯芳香微胶囊的研究. 张永波，高来宝等.天津工业大学学报，第20卷第3期. 2001 |
| 聚氨酯芳香微胶囊的研究. 张永波，高来宝等.天津工业大学学报，第20卷第3期. 2001 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1936170A (en) | 2007-03-28 |
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| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
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| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Jiangyin Ruco Technology Co., Ltd. Assignor: Hua Mingyang Contract fulfillment period: 2009.4.10 to 2014.4.10 contract change Contract record no.: 2009320000804 Denomination of invention: Method for preparing polyurethane fragrant microcapsules Granted publication date: 20080625 License type: Exclusive license Record date: 2009.5.6 |
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| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.4.10 TO 2014.4.10; CHANGE OF CONTRACT Name of requester: JIANGYIN CITY NUOKE SCIENCE CO., LTD. Effective date: 20090506 |
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| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20151211 Address after: 214421 Jiangsu city of Jiangyin province Zhenlong Hua Industrial Zone sand sand road No. 8 Patentee after: Jiangyin city's biological new Mstar Technology Ltd Address before: 214421 Jiangsu city in Jiangyin Province town of Hua Qin Feng Road No. 53 Patentee before: Hua Mingyang |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080625 Termination date: 20150914 |
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| EXPY | Termination of patent right or utility model |