CN1565192A - Monoacid tablet chlorine dioxide disinfectant preparation method - Google Patents
Monoacid tablet chlorine dioxide disinfectant preparation method Download PDFInfo
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- CN1565192A CN1565192A CN 03137084 CN03137084A CN1565192A CN 1565192 A CN1565192 A CN 1565192A CN 03137084 CN03137084 CN 03137084 CN 03137084 A CN03137084 A CN 03137084A CN 1565192 A CN1565192 A CN 1565192A
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Abstract
The invention discloses a monoacid tablet chlorine dioxide disinfectant preparation method, wherein a monobasic powder preparation chlorine dioxide disinfection agent is used as the principal raw material, and a finite proportion of stabilizer, plasticizer, dehydrating agent and releasing agent are charged in and mixed homogeneously under suitable condition of process and environment moisture, the solid tablet disinfectant is prepared on the tablet making machine after pelletization.
Description
Invention field
The present invention relates to the preparation method of a kind of efficient, environmental protection, convenient, safe monobasic tablet disinfection agent of chlorine dioxide, belong to the technology of preparing of strong oxidized form chemosterilant.
Background of invention
Along with the economic development social progress, people's environmental consciousness strengthens day by day, and quality of life progressively improves, and various types of disinfectants more and more are widely used in Human's production and life.According to rough Statistics, at present China is annual consumes ton surplus the disinfectant 200,000, exports 100,000 tons, is worth about 3,000,000,000 yuan.In numerous disinfectants, chlorine dioxide has optimum combination property and economic benefit, is the desirable substitute products of traditional chlorine system disinfectant.
1. chlorine dioxide has the high-efficiency broad spectrum bactericidal property, and its sterilizing ability is 2.6 times of chlorine, kill vegetative forms of bacteria, gemma, fungi, virus etc. fully.Sars coronavirus there is potent killing action.The chlorine dioxide speed of action is fast, and efficacy stability is not influenced by acid-base value in the water, content of organics, has effectively overcome the weakness of chlorine-containing disinfectant to the water quality sensitivity.
2. chlorine dioxide is a strong oxidizer, also has many-sided functions such as deodorizing, bleaching, algae removal, stripping mud, anticorrosion, antitoxin, fresh-keeping, decolouring except that bactericidal property simultaneously, range of application and extensively.
3. The World Health Organization (WHO) confirms, and chlorine dioxide totally nontoxic evil is proposed as the AI level product in the safe disinfection material.Approved chlorine dioxide such as the U.S., Canada, Japan, West Europe are used for food, food processing industry, pharmacy industry, hospital, public environment.Be the generation of " three cause material " (teratogenesis, carcinogenic, mutagenesis) in the control drinking water, the American-European developed country alternative chlorine of extensive use chlorine dioxide carries out drinking water disinfection.It is disinfectant and new food additive that China's health ministry is also ratified chlorine dioxide.
The disinfection agent of chlorine dioxide range of application is extremely extensive, can be used for:
1. drinking water, swimming pool and landscape water, breeding water body, industrial circulating cooling water, production technology are removed algae, hospital, life and industrial sewage wastewater treatment with water sterilization.
2. the sterilization of medicine equipment, diagnosis and treatment articles for use, protective articles: the pipe container sterilization of food processing industry, pharmacy industry removes becomes silted up; Public place public objects such as catering trade, lodging industry, cosmetology industry, toilet, metope ground, clothing fabric, disinfectings such as the vehicles.
3. the disinfecting, deodorizing in spaces such as ward, workshop, storeroom, freezer, refrigerator.
4. disinfectings such as public environment, plague area, infected area, livestock-raising field, military use.
5. the disinfectant fresh-keeping of fruit and vegetable; The sterilization of fresh meat goods is anticorrosion.
6. wash one's hands and other non-surface of a wound skin health sterilizations.
The big industries of wastewater treatment capacity such as its after image papermaking, process hides, pharmacy, chemical industry, smelting, textile printing and dyeing, food processing, petrochemical industry all have wilderness demand to the monobasic tablet disinfection agent of chlorine dioxide that the present invention relates to.
Chlorine dioxide is a gas, the character instability, inflammable and explosive, in order to solve safety, the convenience in its production, the use, people through special compound or the mixture be processed into, at present generally have two types of liquid and solids as what disinfectant used with chlorine dioxide.Fluid product commonly used is a stable ClO 2 solution.Quantitative chlorine dioxide is dissolved in the certain density alkaline solution makes stoste, use the on-the-spot activation of acidic activator (liquid or solid) during application again, instant use (patent).The solid chlorine dioxide product is many to be made up of propellant and activator (solid acid) two components, propellant or chlorite, or make with absorbing process, soon chlorine dioxide or stable solutions are adsorbed on and make (patent) on the porous type solid matter.Liquid or solid product no matter, existing chlorine dioxide all needs two component splits packing, and existing tablet also is to be divided into A sheet, B sheet, all need carry out activation processing (mixing two component 15-20 minutes) during application in advance, and the subject matter of bringing thus is:
1. during chlorine dioxide activation, the chlorine dioxide of the Chan Shenging overpowering odor of emerging has the toxicity and the excitant of similar chlorine suddenly, can encroach on respiratory tract and eyes, when concentration is high, the infringement nervous centralis, severe patient can cause death and die, and admissible concentration is 0.1ppm in air.And activating solution belongs to strong acid, and operating personnel are easily burnt by strong acid, so the operator needs indispensable corresponding professional knowledge, under the good ventilation condition, carries out in suitably airtight nonmetallic vessel.Very easily cause danger during misoperation.
2. the chlorine dioxide product is two a components packing, an acidity, and an alkalescence, if two component haptoreactions, concentration in the air 〉=8% o'clock just very easily produces fierce chemical reaction, causes to fire.So must be strictly on guard against spill and leakage reaction in the accumulating, be strictly on guard against extruding, bump, high temperature, high light or with the organic matter coexistence, in the existing many factories of China with sell and this type of explosive incident took place, cause the heavy losses of lives and properties.
3. during activation act, chlorine dioxide is escaped in a large number, shows according to Chinese Environmental Science Institute data, and loss of effective components is up to 85-90%, and activation efficiency is 10-15% only, causes the significant wastage of product, has improved the working concentration and the disinfection cost of product greatly.
Problem that Rongding Water and Environment Biochemical Techn Co., Ltd., Dingzhou exists in using at chlorine dioxide has been developed the monobasic pulvis disinfection agent of chlorine dioxide new product of overactivity rate, one pack system, unified packing.Product need not activation when using, directly pulvis is sealed off and poured in the water, just can obtain limpid transparent yellow green aqueous solution of chlorine dioxide.Product has kept the premium properties of chlorine dioxide, has overcome many deficiencies of product in the past, makes accumulating, uses and really realized high efficient and reliable, safe and convenient, for vast market prospect has been opened up in the application of chlorine dioxide.
During the patent of invention of the said firm " monobasic pulvis disinfection agent of chlorine dioxide preparation method " is being declared separately and is being accepted.Its inventive principle is: adopt two kinds of water-soluble passivator, make it to be attached to respectively alkaline propellant and acidic active agent particle surface, form one deck passivation coverlay closely, when two components are mixed, can be under a kind of drying regime barrier film each other, can't directly contact.During use, as long as product is soluble in water, passivating film dissolves disappearance at once, and two component haptoreactions discharge chlorine dioxide, forms aqueous solution of chlorine dioxide.Performance requirement to passivator is: strong tackness, strong, soluble in water, the feasible process of absorbent drying function.
Its main summary of the invention is: the manufacture craft aspect is improved, designed water-soluble passivator formula; Development is suitable for passivator RD1, the RD2 of acid and alkali grain respectively; Passivation process are overlapped in design slaking two, are applicable to the Passivation Treatment of alkaline propellant and acidic active agent respectively; Development is dry, passivating technique equipment, makes the reliably coexistence in dry atmosphere of two components, guarantees the safety of product at preparation, packing, storage and transport process; Preferred reliable detection method guarantees product quality.Passivation process has effectively realized propellant and one bag of change packing that activator directly mixes, and has preparation technology's characteristics simple, easy to use, with low cost.
Monobasic pulvis disinfection by chlorine dioxide pulvis safe and convenient, activation rate height, greatly reduce accumulating, use cost, application experiment shows, under equal service condition, the use cost of unified chlorine dioxide only is the 20-25% of stability chlorine dioxide, and is suitable with the use cost of clorox.
But the monobasic powder product of disinfection agent of chlorine dioxide in packing, storing, metering with in using still not as monobasic tablet product come accurately, convenience, safety, commodity be good, so exploitation monobasic tablet disinfection agent of chlorine dioxide product is the active demand in user and market.Yet, because chlorine dioxide is a kind of inflammable and explosive gaseous matter, though be solidificated in the solid, when adopting tablet machine to beat sheet, fire and explosive risks still taking place easily, and be difficult to moulding, does not therefore still have monobasic tablet disinfection agent of chlorine dioxide product to come out so far both at home and abroad.For this reason, the objective of the invention is to make monobasic tablet disinfection agent of chlorine dioxide product, and the preparation method who makes monobasic tablet disinfection agent of chlorine dioxide is provided.
Summary of the invention
The monobasic tablet disinfection agent of chlorine dioxide product that the present invention proposes has convenience of carrying, pack, store and transport, measure and advantage safe in utilization.Although alkaline propellant and acidic activator are wrapped up by water-soluble passivating film, in the process of film-making, the breakage of passivating film takes place probably, thereby the effusion of chlorine dioxide takes place, chlorine dioxide is inflammable and explosive gaseous matter, is easy to cause the accident; Monobasic pulvis chlorine dioxide is beaten sheet difficulty, not easy-formation.The monobasic tablet disinfection agent of chlorine dioxide product that the present invention proposes does not appear in the newspapers so far.
The present invention is by selecting stabilizing agent, desiccant, forming agent, releasing agent, and moisture and the humidity of environment and the pressure of beating sheet of strict control pulvis prepare successful monobasic tablet disinfection agent of chlorine dioxide product.
Technological process of the present invention:
1. select unified chlorine dioxide pulvis.
2. add stabilizing agent, desiccant, forming agent and releasing agent, and evenly mix.
3. granulating is 10 to 20 order particles.
4. machinery is beaten sheet.
The selection of the material of making tablet of the present invention
The monobasic chlorine dioxide pulvis, specification is 40～60 orders, is preferably 60 orders, and the content of chlorine dioxide is 8～10%, is preferably 8%, and shared material gross weight ratio is 20%～50%.Preferred 25% (W/W).
Stabilizing agent can be selected 200 purpose talcum powder, 500 purpose calcium carbonate etc., preferred 500 purpose calcium carbonate.The shared material gross weight ratio of stabilizing agent is 20%～40%, preferred 25% (W/W).
Forming agent can be selected sodium sulphate, magnesium sulfate, citric acid etc., preferably sulfuric acid sodium.The shared material gross weight ratio of forming agent is 20～60%, preferred 40% (W/W).
Desiccant can be selected calcium chloride, silica gel etc., preferably calcium chloride.The shared material gross weight of desiccant is 5～10%, preferred 7.5% (W/W).
Releasing agent can be selected stearic acid compound for example dolomol, zinc stearate, calcium stearate etc., preferred dolomol.
Selection is used for the moisture of the various pulvis of film-making must be less than 0.2% (W/W), preferably less than 0.1% (W/W).
The equipment of making tablet of the present invention is selected
Beat sheet and can select T2P-37 type forming machine, Distributions in Liaocheng of Shandong Province ten thousand is closed industrial Manufacturing Co., Ltd and is produced.
Process conditions when the present invention beats sheet
Envionmental humidity when beating sheet must be less than 40%R.H. preferably less than 30%R.H..
Beating sheet pressure must be less than 4T/cm2, preferred 3.5T/cm
2
Key problem in technology of the present invention is the relative moisture of grain graininess, moisture and the environment of the used pulvis of control film-making, and adds suitable stabilizers, desiccant, forming agent and releasing agent.
Describe in detail
The following example of example is used to illustrate the situation of each side of the present invention.
Example: monobasic tablet chlorine dioxide example of making
In environmental temperature is 15 ℃, relative moisture is under 30% the condition, the moisture of all materials all is lower than under the prerequisite of 0.2% (W/W), (specification is: 50 orders to play the unified chlorine dioxide pulvis that sheet material adopts our company to produce, chlorine dioxide content 8%) 0.25g.: stabilizing agent, zinc stearate (chemical pure, Yangtse River in Chongqing set sail chemical industry Co., Ltd produce) 0.01g; Forming agent, magnesium sulfate (chemical pure is gone up the production of sea green source Fine Chemical Works) 0.4g; Desiccant: calcium chloride (chemical pure, the prosperous chemical plant of Tianjin City Tanggu district China) 0.075g; Releasing agent: calcium carbonate (the prosperous chemical plant of Tianjin City Tanggu district China produces for chemical pure, 500 orders) 0.265g, adopt agitator (V150 type mixing and blending machine, Laizhou City, Shandong dragon Xiang chemical machinery company produces), with the speed of per minute 600 commentaries on classics, evenly stir 12 clocks, until even fully.
In environmental temperature is 15 ℃, and relative moisture is under 30% the condition, with the above-mentioned material that the stirs tablet machine (T2P-37 type forming machine, Distributions in Liaocheng of Shandong Province ten thousand close industrial Manufacturing Co., Ltd and produce) of packing into, with 3.5T/cm
2Pressure under film-making (diameter is 8mm, and thickness is the standard tablet of 4mm, every 1g).The sealed polyethylene plastic bottle of packing into is preserved.
Inspection
The quality inspection of monobasic tablet chlorine dioxide is carried out as follows, and sample is soluble in water, makes yellowish green ClO 2 solution with oxidisability.Chlorine dioxide oxidation potassium iodide makes it discharge iodine, again the iodine of separating out with sodium thiosulfate standard titration solution drop reaction.
(1) reagent and material
A. malonic acid solution: 10%;
B. sulfuric acid solution: C (1/2H
2SO
4)=2mol/L;
C. liquor kalii iodide: 10%;
D. sodium thiosulfate standard titration solution: C (Na
2S
2O
3) be about 0.05mol/L;
E. soluble starch solution 0.5%, and the operating period was two weeks.
(2) analytical procedure
A. quick weighing 12g sample (being accurate to 0.1g) is dissolved in the 1000ml water, be mixed the chlorine dioxide test solution.
B.5min the back places the iodine flask that contains 100ml water with pipette, extract 5ml test solution, adds malonic acid solution 2ml, shakes up.After leaving standstill reaction 2min, add sulfuric acid solution 10mk, liquor kalii iodide 10ml.Cover bottle cap, and behind the shake mixing, add water number and drip, put dark place reaction 5min in iodine flask Gai Yuan.
C. open the iodine flask bottle cap, allow the water that covers edge flow in the bottle.With the 25ml mark look base buret titration that the sodium thiosulfate standard titration solution is housed, free-iodine.Shake while dripping.Treat that solution claims when faint yellow, add 10 of starch solutions, solution becomes blue look immediately.Continue titration to blue decoloration.The total amount of the sodium thiosulfate standard titration solution that record consumes.Replication three times is got its mean value and is calculated.
(3) result calculates
Chlorine dioxide (CLO
2) percentage composition (W) calculate by formula (1):
In the formula: W----chlorine dioxide percentage composition, %;
The concentration of C----sodium thiosulfate standard titration solution, mol/L;
The volume of the sodium thiosulfate standard solution that consumes during the V1---titration, ml;
V2---adds the volume of ClO 2 solution in the iodine flask, ml with pipette;
M----is dissolved in the quality of powdered CLO 2 in the 1000ml water, g;
1mol/L sodium thiosulfate standard solution 1ml is equivalent to the chlorine dioxide of 13.49mg.
(4) allowable error
The arithmetic value of the capable measurement result of making even is that twice parallel determination result's of measurement result relative error is not more than 0.1%.
(5) the experimental result experimental result sees Table 1
Table 1
| Sample number into spectrum | ?????1 | ?????2 | ?????3 | ?????4 | Mean value |
| Chlorine dioxide content | ????8.3％ | ????8.2％ | ????8.1％ | ????8.4％ | ????8.25％ |
(6) tablet stores experiment
Preserved 3 months in the sealing of sealed polyethylene plastic bottle, tablet does not have efflorescence, smooth surface.Again carrying out chlorine dioxide content detects.
Table 2
| Sample number into spectrum | ?????1 | ?????2 | ?????3 | ?????4 | On average |
| Chlorine dioxide content | ????8.2％ | ????8.2％ | ????8.1％ | ????8.3％ | ????8.20％ |
From the data of table 2 and table 1 as can be known, the basic no change of the content of chlorine dioxide.
Claims (10)
1. monobasic tablet disinfection agent of chlorine dioxide product.
2. the fabrication material package of the described monobasic tablet of claim 1 disinfection agent of chlorine dioxide product is drawn together monobasic pulvis chlorine dioxide, stabilizing agent, desiccant, forming agent and releasing agent.
3. the described monobasic pulvis of claim 2 chlorine dioxide specification is 40～60 orders, is preferably 60 orders; The content of chlorine dioxide is 8～10% in the pulvis, preferred 8%.The gross weight ratio of the described material of shared claim 2 is 20%～50%.Preferred 25% (W/W).
4. the described stabilizing agent of claim 2 is 200 purpose talcum powder or 500 purpose calcium carbonate etc., preferred 500 purpose calcium carbonate.The gross weight ratio of the said material of the shared claim 2 of stabilizing agent is 20%～40%, preferred 50% (W/W).
5. the described releasing agent of claim 2 is a stearate, comprises dolomol, zinc stearate, calcium stearate etc., but is not limited to these stearate, preferred dolomol.
6. the described forming agent of claim 2 can be sodium sulphate, magnesium sulfate, citric acid etc., preferably sulfuric acid sodium.The shared gross weight ratio of forming agent is 10～20%, preferred 15% (W/W).
7. the described desiccant of claim 2 is calcium chloride, silica gel etc., preferably calcium chloride.The shared material gross weight of desiccant is 5～10%, preferred 7.5% (W/W).
8. the moisture of the described various materials of claim 2 must 0.2% (W/W), preferably less than 0.1% (W/W).
9. must must carry out abundant mixing under preferably less than the condition of 30%R.H less than 40%R.H. at envionmental humidity according to the material of claim 2,3,4,5,6,7 requirement, and at T2P-37 type forming machine, Distributions in Liaocheng of Shandong Province ten thousand is closed on the tablet machine that industrial Manufacturing Co., Ltd produces and is made the described monobasic tablet of claim 1 disinfection agent of chlorine dioxide product.
10. when carrying out film-making according to claim 8, the sheet pressure of beating of pelleter must be less than 4T/cm
2, preferred 3.5T/cm
2
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03137084 CN1565192A (en) | 2003-06-18 | 2003-06-18 | Monoacid tablet chlorine dioxide disinfectant preparation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101228868B (en) * | 2008-02-27 | 2010-06-09 | 河北科技大学 | Unitary solid chlorine dioxide effervescent tablet and preparation method thereof |
| CN104995133A (en) * | 2013-03-29 | 2015-10-21 | 大曹株式会社 | Tablet for preparing solution of chlorine dioxide |
| CN108079359A (en) * | 2017-12-22 | 2018-05-29 | 浙江惠普科技发展有限公司 | A kind of steam atomization air purification bag |
| CN111226980A (en) * | 2020-03-28 | 2020-06-05 | 晋玮璘 | Reactive chlorine dioxide solid preparation and preparation method thereof |
-
2003
- 2003-06-18 CN CN 03137084 patent/CN1565192A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101228868B (en) * | 2008-02-27 | 2010-06-09 | 河北科技大学 | Unitary solid chlorine dioxide effervescent tablet and preparation method thereof |
| CN104995133A (en) * | 2013-03-29 | 2015-10-21 | 大曹株式会社 | Tablet for preparing solution of chlorine dioxide |
| CN108079359A (en) * | 2017-12-22 | 2018-05-29 | 浙江惠普科技发展有限公司 | A kind of steam atomization air purification bag |
| CN111226980A (en) * | 2020-03-28 | 2020-06-05 | 晋玮璘 | Reactive chlorine dioxide solid preparation and preparation method thereof |
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