CN100392175C - Method for producing polyurothane antibiotic aromatic micro-capsule - Google Patents
Method for producing polyurothane antibiotic aromatic micro-capsule Download PDFInfo
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- CN100392175C CN100392175C CNB2006100960393A CN200610096039A CN100392175C CN 100392175 C CN100392175 C CN 100392175C CN B2006100960393 A CNB2006100960393 A CN B2006100960393A CN 200610096039 A CN200610096039 A CN 200610096039A CN 100392175 C CN100392175 C CN 100392175C
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Abstract
The present invention relates to a preparation method of polyurethane anti-bacterial aromatic microcapsule. Its raw material includes oil phase and water phase, in which the oil phase is formed from polyisocyanate, essence, inorganic anti-bacterial agent and cyclohexane, and the water phase is composed of sodium hydroxide, sodium alginate and deionized water. Its preparation method includes the following several steps: adding polyethylene glycol and acetone into oil phase, mixing them and drop-adding the obtained mixture into water phase for 1.5-2hr, stirring speed is 400-600 rpm at 40-60deg.C, after the drop-addition is completed, heating to 50-70deg.C, making reaction for 1-1.5hr, filtering the obtained product so as to obtain the invented product white emulsion. The grain size of said microcapsule prepared by using the invented method is 20-4 micrometers.
Description
Technical field
The present invention relates to a kind of weaving aromatic micro-capsule, especially relate to a kind of preparation of polyurothane antibiotic aromatic micro-capsule.
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.Because there is the cyst wall instability in it, problems such as porosity is irregular, therefore its slow release is not high, spices fragrance remaining time with its parcel is short, and these materials adopt the preparation of oiliness system mostly, and some monomer free does not meet environmental requirement sometimes, and do not have antibacterial functions, be easy to breed bacteria and lost efficacy.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, provide a kind of fragrance slow release higher, environmentally friendly, have the preparation method of preparation of the polyurothane antibiotic aromatic micro-capsule of antibacterial functions.
The object of the present invention is achieved like this: a kind of preparation method of polyurothane antibiotic aromatic micro-capsule is characterized in that: the oil phase of the preparation material of polyurothane antibiotic aromatic micro-capsule is made up of polyisocyanates, essence, inorganic antiseptic 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
Inorganic antiseptic 1～2g
Cyclohexane 20～25ml;
Water:
15% NaOH 2ml
Sodium alginate 0.3g
Deionized water 200ml;
Polyethylene glycol 3.0g.
Polyisocyanates of the present invention can be IPDI, TDI or HDI.
Inorganic antiseptic of the present invention can be nano silicon oxide, titanium oxide or the basic zirconium phosphate of load silver ion, zinc ion; Molecular weight polyethylene glycol 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, and the aromatic micro-capsule fragrance slow release that obtains is higher, environmentally friendly and environmental protection, and the capsule material has certain resilience, is easy to processing; Add inorganic antiseptic, make product have antibacterial functions, these microcapsules are to Escherichia coli, staphylococcus aureus, and Candida albicans has extremely strong antibacterial ability.
The specific embodiment
Polyurothane antibiotic aromatic micro-capsule of the present invention is by spices, inorganic antiseptic and be wrapped in outer polyurethane and constitute.Its preparation method is as follows:
Embodiment 1:
One, gets the raw materials ready
Oil phase: IPDI3.33g, cream jasmin france 19g carries silver-colored silica 1g, 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 carries silver-colored titanium oxide 1.5g, cyclohexane 25ml
Water: NaOH (15%) 2ml, deionized water: 200ml, sodium alginate: the polyethylene glycol 3.0g of 0.3g 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 (4)
1. the preparation method of a polyurothane antibiotic aromatic micro-capsule, it is characterized in that: the oil phase of the preparation material of polyurothane antibiotic aromatic micro-capsule is made up of polyisocyanates, essence, inorganic antiseptic 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
Inorganic antiseptic 1～2g
Cyclohexane 20～25ml
Water:
15% NaOH 2ml
Sodium alginate 0.3g
Deionized water 200ml;
Polyethylene glycol 3.0g.
2. the preparation method of a kind of polyurothane antibiotic aromatic micro-capsule according to claim 1, it is characterized in that: described polyisocyanates is IPDI, TDI or HDI.
3. the preparation method of a kind of polyurothane antibiotic aromatic micro-capsule according to claim 1 and 2, it is characterized in that: described inorganic antiseptic is nano silicon oxide, titanium oxide or the basic zirconium phosphate of load silver ion, zinc ion.
4. the preparation method of a kind of polyurothane antibiotic aromatic micro-capsule 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 |
|---|---|---|---|
| CNB2006100960393A CN100392175C (en) | 2006-09-14 | 2006-09-14 | Method for producing polyurothane antibiotic aromatic micro-capsule |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100960393A CN100392175C (en) | 2006-09-14 | 2006-09-14 | Method for producing polyurothane antibiotic aromatic micro-capsule |
Publications (2)
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| CN1932138A CN1932138A (en) | 2007-03-21 |
| CN100392175C true CN100392175C (en) | 2008-06-04 |
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| CNB2006100960393A Expired - Fee Related CN100392175C (en) | 2006-09-14 | 2006-09-14 | Method for producing polyurothane antibiotic aromatic micro-capsule |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103211331A (en) * | 2013-05-06 | 2013-07-24 | 中国热带农业科学院南亚热带作物研究所 | Antibacterial and anti-inflammation lubricative glove containing natural cinnamyl aldehyde and manufacturing method thereof |
| CN103360731B (en) * | 2013-07-04 | 2017-09-12 | 江苏中杰澳新材料有限公司 | A kind of microencapsulation terylene fragrant masterbatch and its manufacture method |
| CN104823996A (en) * | 2015-05-13 | 2015-08-12 | 山东农业大学 | Preparation method of pyraclostrobin microcapsules |
| CN107603190A (en) * | 2017-09-21 | 2018-01-19 | 河南驼人医疗器械集团有限公司 | A kind of medical antibacterial polyurethane material and preparation method thereof |
| CN112029510B (en) * | 2020-10-15 | 2021-09-17 | 丽水学院 | Composite soil conditioner and preparation method and application thereof |
| CN113171753B (en) * | 2021-04-27 | 2022-01-28 | 西南科技大学 | Preparation of sodium alginate-zirconium phosphate composite beads and adsorption application of sodium alginate-zirconium phosphate composite beads in nuclear waste liquid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07118439A (en) * | 1993-10-27 | 1995-05-09 | Toru Yamamoto | Microcapsule composition of lower cyclic alkane |
| US5962003A (en) * | 1998-03-30 | 1999-10-05 | Council Of Scientific & Industrial Research | Process for the preparation of polyurethane microcapsules containing monocrotophos |
| US6123988A (en) * | 1998-06-12 | 2000-09-26 | Council Of Scientific & Industrial Research | Process for the preparation of polyurethane spherical particle |
-
2006
- 2006-09-14 CN CNB2006100960393A patent/CN100392175C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07118439A (en) * | 1993-10-27 | 1995-05-09 | Toru Yamamoto | Microcapsule composition of lower cyclic alkane |
| US5962003A (en) * | 1998-03-30 | 1999-10-05 | Council Of Scientific & Industrial Research | Process for the preparation of polyurethane microcapsules containing monocrotophos |
| US6123988A (en) * | 1998-06-12 | 2000-09-26 | Council Of Scientific & Industrial Research | Process for the preparation of polyurethane spherical particle |
Non-Patent Citations (6)
| Title |
|---|
| 环己烷对相变材料微胶囊结构与性能的影响. 王学晨，张兴祥，樊耀峰，牛建津，蔡利海.天津工业大学学报，第23卷第4期. 2004 |
| 环己烷对相变材料微胶囊结构与性能的影响. 王学晨，张兴祥，樊耀峰，牛建津，蔡利海.天津工业大学学报，第23卷第4期. 2004 * |
| 聚氨酯芳香微胶囊的研究. 张永波，高来宝，曹虹霞，张涛.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，曹虹霞，张涛.天津工业大学学报，第20卷第3期. 2001 * |
| 芳香整理用聚氨酯微胶囊的研制. 张永波，高来宝，曹虹霞，张涛.针织工业，第4期. 2002 |
| 芳香整理用聚氨酯微胶囊的研制. 张永波，高来宝，曹虹霞，张涛.针织工业，第4期. 2002 * |
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Assignee: Jiangyin Ruco Technology Co., Ltd. Assignor: Hua Mingyang Contract fulfillment period: 2009.4.10 to 2014.4.10 contract change Contract record no.: 2009320000796 Denomination of invention: Method for producing polyurothane antibiotic aromatic micro-capsule Granted publication date: 20080604 License type: Exclusive license Record date: 2009.5.6 |
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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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