CN1820607A - Process for preparing chlorine dioxide slow-release micro capsule - Google Patents
Process for preparing chlorine dioxide slow-release micro capsule Download PDFInfo
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- CN1820607A CN1820607A CN 200610025332 CN200610025332A CN1820607A CN 1820607 A CN1820607 A CN 1820607A CN 200610025332 CN200610025332 CN 200610025332 CN 200610025332 A CN200610025332 A CN 200610025332A CN 1820607 A CN1820607 A CN 1820607A
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- chlorine dioxide
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- micro capsule
- microcapsules
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Abstract
The process of preparing slow-released chlorine dioxide microcapsule includes the following steps: 1. mixing chlorine dioxide aqua and beta-cyclodextrin in the mass ratio of 1 to 2-10 at 0-20deg.c through stirring; and 2. drying at 20-60deg.c for 0.5-5 hr and grinding. The microcapsule has its core separated from outside and not affected by outer humidity, oxygen, ultraviolet ray, etc. and the present invention adopts microcapsule technology in preparing disinfectant and stabilized chlorine dioxide.
Description
Technical field
The present invention relates to a kind of preparation method of microcapsules, belong to the fine chemical technology field, particularly relate to a kind of preparation method of chlorine dioxide microcapsules.
Background technology
Chlorine dioxide is one of good disinfectant, and it is obtaining general application as disinfectant, oxidant, biocide, algicide, bleaching agent, eliminating smell agent, cleaning agent in its association area.Since chlorine dioxide comes out, successively to be used to the water body disinfection in sterilization, food wrapper sterilization and bleaching, water flood recovery and de-plugging of well, health and epidemic prevention sterilization, grease-decolor and flour in paper pulp and fiber bleached, drinking water disinfection, food processing, meat fruit and vegetable and aquatic products sterilization and fresh-keeping, industrial colling and wastewater treatment, the clinical treatment and the bleaching in the rice processing and sterilization, the aquaculture and to prevent and cure diseases and water factory kills algae and control biological pollution and pipeline and all many-sides such as silts up.Chlorine dioxide is accepted by the user and is approved, is a kind of up-and-coming disinfectant.
But the chlorine dioxide instability is heated or is met light and easily resolves into oxygen and chlorine, sets off an explosion.In the air volume fraction greater than 10% or water in concentration all low-level blast can take place during greater than 100g/L.In the presence of organic steam, it is strong that this blast may become.No matter compression and all trials of storing chlorine dioxide are separately or with other gas combinations, in commercial all not successes, because its explosion danger, chlorine dioxide must be made in the place to use.It is safer less than 10% o'clock that the gas chlorine dioxide is diluted to volume fraction with air; The concentration of aqueous solution of chlorine dioxide is lower than about 8g/L～10g/L, will not produce the dangerous high-vapor-pressure that enough sets off an explosion.In the practice of water treatment, the concentration of chlorine dioxide seldom surpasses 4g/L, and processing horizontal is generally in 0.1g/L arrives the such scope of 5.0mg/L.
Just because of this lability of chlorine dioxide, it is very restricted on using.Seek a kind of effective means the chlorine dioxide stabilisation is just seemed particularly important.
Microcapsules technology is that a kind of filmogen of using coats solid or liquid, makes it form the technology of fine particle.The fine particle that obtains is microcapsules, and the size of general particle is in micron or millimeter scope.
The material that wraps in microcapsules inside is called the capsule heart, and the capsule heart can be a solid, also can be liquid or gas.The coating film that the microcapsules outside is formed by filmogen is called the wall material.The wall material is normally formed by macromolecular material natural or that synthesize, also may be inorganic compound.According to character, the purposes difference of the capsule heart, can adopt one or more wall materials to coat.
When the advantage of microcapsules technology was to form microcapsules, the capsule heart was isolated with external environment by coating, and its character can remain with having no effect, and under suitable condition, can discharge from the wall material again.This brings many facilities to use.Behind liquid formation microcapsules, become pressed powder, this all brings great convenience for its use, transportation, storage.
If the wall material of selecting for use has semi permeability, then the liquid capsule heart or the water-soluble capsule heart can be by the processes of dissolving, infiltration, diffusion, see through membranous wall and discharge, and the chemical composition that rate of release can be by changing the wall material, thickness, hardness, pore size etc. are controlled.This microcapsules with sustained release speed function are particularly useful in the application of aspects such as perfume, medicine, agricultural chemicals.In a word, microcapsules technology has been subjected to the attention of all trades and professions.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of chlorine dioxide slow-release micro capsule, adopts beta-schardinger dextrin-as the wall material, and the method formation microcapsules by physics to remedy the deficiencies in the prior art, meet the demands of production and living.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of preparation method of chlorine dioxide slow-release micro capsule comprises the steps:
(1) under 0 ℃～20 ℃ temperature, be that 1: 2～10 aqueous solution of chlorine dioxide mixes with beta-schardinger dextrin-with mass ratio, fully stir;
(2) dry 0.5h～5h discharging under 20 ℃～60 ℃ temperature, grinding.
As optimized technical scheme: described aqueous solution of chlorine dioxide is under vacuum condition, the concentrated sulfuric acid is added drop-wise in the solution of chloracid potassium and oxalic acid, generates yellow green chlorine dioxide body and function frozen water and absorbs and make.
Being ground to granularity in the step (2) is 200um～500um.
The invention has the beneficial effects as follows: the microcapsules of making, the capsule heart separates with external environment, just can make the influence of factors such as its humidity of avoiding the external world, oxygen, ultraviolet ray, thereby the unsettled capsule heart of character is undergone no deterioration, microcapsules technology is applied on the disinfectant, and the characteristic of utilizing microcapsules is with the chlorine dioxide stabilisation.
Embodiment
Below in conjunction with specific embodiment the present invention is further elaborated.
Embodiment 1
Under vacuum condition, the concentrated sulfuric acid is added drop-wise in the solution of chloracid potassium and oxalic acid, generate the yellow green chlorine dioxide, make aqueous solution of chlorine dioxide 30 grams with the frozen water absorption, under 20 ℃, be added drop-wise in the beta-schardinger dextrin-of 90 grams, stir, in 50 ℃ of dryings 1.5 hours, being ground to granularity was 200um, test its release performance, can obtain the slow released ClO 2 microcapsule product.
Embodiment 2
Under vacuum condition, the concentrated sulfuric acid is added drop-wise in the solution of chloracid potassium and oxalic acid, generates the yellow green chlorine dioxide, make aqueous solution of chlorine dioxide 20 grams with the frozen water absorption, under 0 ℃, be added drop-wise in the beta-schardinger dextrin-s of 40 grams, stir, in 20 ℃ of dryings 5 hours, stored 1 month in 0 ℃, being ground to granularity is 500um, tests its release performance, obtains the slow released ClO 2 microcapsule product.
Embodiment 3
Under vacuum condition, the concentrated sulfuric acid is added drop-wise in the solution of chloracid potassium and oxalic acid, generate the yellow green chlorine dioxide, make aqueous solution of chlorine dioxide 20 grams with the frozen water absorption, under 0 ℃, be added drop-wise in the beta-schardinger dextrin-of 200 grams, stir, in 60 ℃ of dryings 0.5 hour, being ground to and being milled to granularity was 300um, test its release performance, can obtain the slow released ClO 2 microcapsule product.
Claims (3)
1, a kind of preparation method of chlorine dioxide slow-release micro capsule is characterized in that comprising the steps:
(1) under 0 ℃～20 ℃ temperature, be that 1: 2～10 aqueous solution of chlorine dioxide mixes with beta-schardinger dextrin-with mass ratio, fully stir;
(2) dry 0.5h～5h discharging under 20 ℃～60 ℃ temperature, grinding.
2, preparation method according to claim 1 is characterized in that: described aqueous solution of chlorine dioxide is under vacuum condition, the concentrated sulfuric acid is added drop-wise in the solution of chloracid potassium and oxalic acid, generates the yellow green chlorine dioxide, makes with the frozen water absorption.
3, preparation method according to claim 1 is characterized in that: being ground to granularity in the step (2) is 200um～500um.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610025332 CN1820607A (en) | 2006-03-31 | 2006-03-31 | Process for preparing chlorine dioxide slow-release micro capsule |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610025332 CN1820607A (en) | 2006-03-31 | 2006-03-31 | Process for preparing chlorine dioxide slow-release micro capsule |
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| CN1820607A true CN1820607A (en) | 2006-08-23 |
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| CN 200610025332 Pending CN1820607A (en) | 2006-03-31 | 2006-03-31 | Process for preparing chlorine dioxide slow-release micro capsule |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009026014A1 (en) * | 2007-08-23 | 2009-02-26 | Ken Harrison | Compositions, systems, and/or methods involving chlorine dioxide ('cio2') |
| CN101810872A (en) * | 2009-12-22 | 2010-08-25 | 北京欧凯纳斯科技有限公司 | Sterilizing and oil-removing multipurpose cloth for kitchens |
| CN102657156A (en) * | 2012-04-13 | 2012-09-12 | 西南林业大学 | Preparation of beta-cyclodextrin sustained-release microcapsule of forestry insect repellant (E)-2-hexenal and determination method |
| CN102669176A (en) * | 2012-05-30 | 2012-09-19 | 吕永生 | Slow-release chlorine dioxide solid disinfectant |
| EP2508474A1 (en) * | 2011-04-08 | 2012-10-10 | Wacker Chemie AG | Composition comprising an alpha-cyclodextrin-chlorine dioxide complex and an inert substance, and also method for production thereof |
| US8563046B2 (en) | 2007-08-23 | 2013-10-22 | Dharma IP, LLC | Compositions, systems, and/or methods involving chlorine dioxide (“ClO2”) |
| CN104273169A (en) * | 2014-09-19 | 2015-01-14 | 中国检验检疫科学研究院 | Solid chlorine dioxide controlled-release disinfectant and preparation method thereof |
| US9073754B2 (en) | 2008-05-30 | 2015-07-07 | Dharma IP, LLC | Systems, methods, and compositions involving chlorine dioxide and zeolite |
| CN106472960A (en) * | 2016-10-20 | 2017-03-08 | 广州市和兴隆食品科技股份有限公司 | A kind of chlorine dioxide stable and preparation method and thimerosal prepared therefrom |
| CN111436426A (en) * | 2020-05-11 | 2020-07-24 | 北京首创股份有限公司 | Secondary chlorination capsule for water delivery of water supply pipeline and preparation method thereof |
| US10850981B2 (en) | 2017-04-25 | 2020-12-01 | Ica Trinova, Llc | Methods of producing a gas at a variable rate |
| EP3618613A4 (en) * | 2017-05-05 | 2021-01-20 | Pamel, Gregory J. | Composition containing chlorine dioxide and methods for using same |
| CN115590020A (en) * | 2022-09-23 | 2023-01-13 | 王世锋（Cn） | Slow-release chlorine dioxide microcapsule taking foam as shell material and preparation method thereof |
| US11912568B2 (en) | 2018-03-14 | 2024-02-27 | Ica Trinova, Llc | Methods of producing a gas at a controlled rate |
-
2006
- 2006-03-31 CN CN 200610025332 patent/CN1820607A/en active Pending
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8563046B2 (en) | 2007-08-23 | 2013-10-22 | Dharma IP, LLC | Compositions, systems, and/or methods involving chlorine dioxide (“ClO2”) |
| EP2223890A3 (en) * | 2007-08-23 | 2010-12-01 | Ken Harrison | Composition, System, and/or Methods Involving Chlorine Dioxide ( CIO2 ) |
| WO2009026014A1 (en) * | 2007-08-23 | 2009-02-26 | Ken Harrison | Compositions, systems, and/or methods involving chlorine dioxide ('cio2') |
| JP2010536861A (en) * | 2007-08-23 | 2010-12-02 | ハリソン，ケン | Compositions, systems, and / or methods with chlorine dioxide (ClO2) |
| US7935271B2 (en) | 2007-08-23 | 2011-05-03 | Ken Harrison | Compositions, systems, and/or methods involving chlorine dioxide |
| AU2008289270B2 (en) * | 2007-08-23 | 2011-09-15 | Dharma IP, LLC | Compositions, systems, and/or methods involving chlorine dioxide ("C1O2") |
| US9073754B2 (en) | 2008-05-30 | 2015-07-07 | Dharma IP, LLC | Systems, methods, and compositions involving chlorine dioxide and zeolite |
| CN101810872A (en) * | 2009-12-22 | 2010-08-25 | 北京欧凯纳斯科技有限公司 | Sterilizing and oil-removing multipurpose cloth for kitchens |
| CN101810872B (en) * | 2009-12-22 | 2013-02-27 | 北京欧凯纳斯科技有限公司 | Sterilizing and oil-removing multipurpose cloth for kitchens |
| EP2508474A1 (en) * | 2011-04-08 | 2012-10-10 | Wacker Chemie AG | Composition comprising an alpha-cyclodextrin-chlorine dioxide complex and an inert substance, and also method for production thereof |
| CN102657156A (en) * | 2012-04-13 | 2012-09-12 | 西南林业大学 | Preparation of beta-cyclodextrin sustained-release microcapsule of forestry insect repellant (E)-2-hexenal and determination method |
| CN102669176A (en) * | 2012-05-30 | 2012-09-19 | 吕永生 | Slow-release chlorine dioxide solid disinfectant |
| CN104273169A (en) * | 2014-09-19 | 2015-01-14 | 中国检验检疫科学研究院 | Solid chlorine dioxide controlled-release disinfectant and preparation method thereof |
| CN106472960A (en) * | 2016-10-20 | 2017-03-08 | 广州市和兴隆食品科技股份有限公司 | A kind of chlorine dioxide stable and preparation method and thimerosal prepared therefrom |
| US10850981B2 (en) | 2017-04-25 | 2020-12-01 | Ica Trinova, Llc | Methods of producing a gas at a variable rate |
| US11518676B2 (en) | 2017-04-25 | 2022-12-06 | Ica Trinova Llc | Methods of producing a gas at a variable rate |
| EP3618613A4 (en) * | 2017-05-05 | 2021-01-20 | Pamel, Gregory J. | Composition containing chlorine dioxide and methods for using same |
| US10925894B2 (en) | 2017-05-05 | 2021-02-23 | Gregory J. PAMEL | Composition containing chlorine dioxide and methods for using same |
| US11912568B2 (en) | 2018-03-14 | 2024-02-27 | Ica Trinova, Llc | Methods of producing a gas at a controlled rate |
| CN111436426A (en) * | 2020-05-11 | 2020-07-24 | 北京首创股份有限公司 | Secondary chlorination capsule for water delivery of water supply pipeline and preparation method thereof |
| CN111436426B (en) * | 2020-05-11 | 2022-04-08 | 北京首创股份有限公司 | Secondary chlorination capsule for water delivery of water supply pipeline and preparation method thereof |
| CN115590020A (en) * | 2022-09-23 | 2023-01-13 | 王世锋（Cn） | Slow-release chlorine dioxide microcapsule taking foam as shell material and preparation method thereof |
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