CN107821405A - A kind of ketone liquid preparation of 1,2 benzisothiazole of low alkali value 3 and preparation method - Google Patents
A kind of ketone liquid preparation of 1,2 benzisothiazole of low alkali value 3 and preparation method Download PDFInfo
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- CN107821405A CN107821405A CN201711192056.1A CN201711192056A CN107821405A CN 107821405 A CN107821405 A CN 107821405A CN 201711192056 A CN201711192056 A CN 201711192056A CN 107821405 A CN107821405 A CN 107821405A
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- low alkali
- alkali value
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- value bit
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
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- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
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- Agricultural Chemicals And Associated Chemicals (AREA)
- Thiazole And Isothizaole Compounds (AREA)
Abstract
The invention discloses a kind of ketone liquid preparation of 1,2 benzisothiazole of low alkali value 3 and preparation method, affiliated industrial bio biocide preparation field.A kind of ketone liquid preparation of 1,2 benzisothiazole of low alkali value 3, is made up of the component of following weight proportion：1,2 benzisothiazole 3 ketone 15.0wt%~30.0wt%, soluble carrier 30.0wt%~60.0wt%, nucleopilic reagent 0.2wt%~1.2wt%, catalyst 0.5wt~1.2wt%, deionized water 20.0wt%~30.0wt%.This kind of ketone liquid preparation of 1,2 benzisothiazole of low alkali value 3 has bactericidal activity height, alkaline low, good water solubility, low-temperature resistance, good dispersion, low cost and other advantages, and invented technology is simple, no coupling product.
Description
Technical field
The present invention relates to industrial bio biocide preparation field, and in particular to a kind of low alkali value 1,2- benzisothiazoles -3-
Ketone liquid preparation.
Background technology
1,2- benzisothiazole-3-ketones (hereinafter referred to as BIT) are a kind of environmentally friendly, widely used industrial bio sterilizations
Agent, suitable for numerous industries such as metal working fluids, emulsion, paint, construction material, leather, paint, agricultural.1,2- benzisoxas
Solubility of the thiazoline -3- ketone in water is low, not easy to operate, the BIT provided with high aqueous solution
For having good advantage in above-mentioned various specific areas.
At present, many BIT liquid preparations are used as using alkali metal hydroxide and neutralized
It is prepared by agent.Chinese patent CN96108878.8 discloses a kind of BIT liquid system, and the patent uses will
The technique of the alkali metal salt of solvent that 1,2- benzisothiazole-3-ketones are configured to one or more and dissolved each other.In embodiment 1
The BIT of 19.3 parts of description and 12 parts of 50%NaOH form BIT sodium salt,
Wherein NaOH is excessive, and formula pH is too high.Too high pH can limit its application, and have corrosivity, shadow to metal
The service life of equipment is rung, if solidification phenomenon occurs in addition latex.
Chinese patent CN201280029122.2 discloses a kind of aqueous solution of BIT, and this is special
Profit is without VOC, glycerine, glycerol derivatives, glycol and/or diol, derivatives and including at least a kind of water-soluble
The biocide of property form.Although the patent use without VOC, glycerine, glycerol derivatives, glycol and/
Or diol, derivatives, neutralized using alkalinous metal, while the method for complex compound is added to reduce pH value, but it is the increase in production
Cost, due to the presence of no cosolvent, the aqueous solution of the BIT of high concentration be difficult to, it is necessary to
It is used cooperatively with other biological agent for killing, further increases cost.
The content of the invention
It is an object of the invention to overcome deficiency of the prior art, according to BIT (1,2-
Benzisothiazolin-3-One chemical structural formula) is shown in Fig. 1, has highly polar group：Carbonyl (C δ +=O δ -), ketone thing
The oxygen atom of carbonyl has electronegativity in matter, can form stronger hydrogen bond with hydrone, but with the increase of carbon number,
Water solubility reduces, more than C6 ketone characteristic substantially not soluble in water, using the group with high-hydrophilic, slightly alkaline in catalyst
In the presence of add on the carbonyl on BIT, you can obtain low alkali value 1,2- benzisothiazoles-
3- ketone liquid preparations, reaction equation are shown in Fig. 2.
The technical scheme is that：
A kind of low alkali value BIT liquid preparation, is made up of the component of following weight proportion：1,2-
Benzisothiazole-3-ketone 15.0wt%~30.0wt%, soluble carrier 30.0wt%~60.0wt%, nucleopilic reagent
0.2wt%~1.2wt%, catalyst 0.5wt~1.2wt%, deionized water 20.0wt%~30.0wt%.
The soluble carrier is polyalcohol or polyol derivative, and it can keep the stability that product has had and divide
Property is dissipated, can be specifically ethylene glycol, propyl alcohol, propane diols, glycerine, glycerine polymer, dipropylene glycol, two propyl alcohol etc..
The nucleopilic reagent is sulfonate, and it can be in lauryl sulfonic acid amine, a- olefin sulfonic acids amine, acesulfame potassium
Any one.
The catalyst is carboxylic acids catalyst, can accelerate the progress of reaction, while is also low alkali value reagent, while carboxylic acid
Class catalyst can be citric acid, ethylenediamine tetra-acetic acid, phytic acid and/or gluconic acid.
The deionized water resistivity is more than 0.5M Ω cm
A kind of preparation method of low alkali value BIT liquid preparation, is comprised the following steps that：
(1) weigh respectively as requested 1,2- benzisothiazole-3-ketones, nucleopilic reagent, soluble carrier, catalyst,
Deionized water；
(2) load weighted soluble carrier, nucleopilic reagent are sequentially added in four mouthfuls of reactors, is stirred under 150rpm rotating speed
Mix, and then warming-in-water adds BIT to 40-50 DEG C, continue 150rpm and be dispersed with stirring 30min；
(3) catalyst is equably added dropwise in the reactor of step (2), time for adding is 0.5 hour, and reaction temperature exists
55-60 DEG C, after being added dropwise to complete, stirring reaction 5 hours；
(4) add deionized water to continue after reacting 1 hour, be down to room temperature, obtain low alkali value 1,2- benzisothiazoles -3-
Ketone liquid preparation.
The low alkali value BIT liquid preparation is weak yellow liquid, and pH is 7.0~8.5.
Beneficial effects of the present invention：
1st, the present invention adds to 1,2- benzisoxas using the group with high-hydrophilic, slightly alkaline in the presence of catalyst
On carbonyl on thiazoline -3- ketone, obtain low alkali value BIT this kind of method of liquid preparation and do not change
The active structure of BIT, there is the characteristics of bactericidal activity is high, alkalescence is low, good water solubility.
2nd, the obtained low alkali value 1,2- benzisothiazole-3-ketone liquid preparations of the present invention have low-temperature resistance, good dispersion,
Low cost and other advantages, and invented technology is simple, no coupling product.
Brief description of the drawings
Fig. 1 is the chemical structural formula of 1,2- benzisothiazole-3-ketones；
Fig. 2 is reaction equation
Fig. 3 control groups survey qualitative data
The low alkali value 1,2- benzisothiazole-3-ketones liquid preparation actual measurement qualitative data of Fig. 4 present invention
Embodiment
Below by non-limiting example, the present invention is expanded on further, understands the present invention.
Embodiment 1
A kind of preparation method of low alkali value BIT liquid preparation, is comprised the following steps that：
(1) BIT 15.0wt%, ethylene glycol 30.0wt%, a- alkene are weighed respectively as requested
Base sulfanilic acid 0.2wt%, citric acid 0.5wt%, deionized water 20.0wt%；
(2) load weighted ethylene glycol, a- olefin sulfonic acid amine are sequentially added in four mouthfuls of reactors, is stirred under 150rpm rotating speed
Mix, and then warming-in-water adds BIT to 40-50 DEG C, continue 150rpm and be dispersed with stirring 30min；
(3) citric acid is equably added dropwise in the reactor of step (2), time for adding is 0.5 hour, and reaction temperature exists
55-60 DEG C, after being added dropwise to complete, stirring reaction 5 hours；
(4) add deionized water to continue after reacting 1 hour, be down to room temperature, obtain low alkali value 1,2- benzisothiazoles -3-
Ketone liquid preparation.
The low alkali value BIT liquid preparation is weak yellow liquid, and pH is 7.0~8.5.
Embodiment 2
A kind of preparation method of low alkali value BIT liquid preparation, is comprised the following steps that：
(1) BIT 21.0wt%, glycerine 55.0wt%, lauryl are weighed respectively as requested
Sulfanilic acid 0.3wt%, gluconic acid 1.0wt%, deionized water 22.7wt%；
(2) load weighted glycerine, lauryl sulfonic acid amine are sequentially added in four mouthfuls of reactors, is stirred under 150rpm rotating speed
Mix, and then warming-in-water adds BIT to 40-50 DEG C, continue 150rpm and be dispersed with stirring 30min；
(3) gluconic acid is equably added dropwise in the reactor of step (2), time for adding is 0.5 hour, reaction temperature
At 55-60 DEG C, after being added dropwise to complete, stirring reaction 5 hours；
(4) add deionized water to continue after reacting 1 hour, be down to room temperature, obtain low alkali value 1,2- benzisothiazoles -3-
Ketone liquid preparation.
The low alkali value BIT liquid preparation is weak yellow liquid, and pH is 7.0~8.5.
Embodiment 3
A kind of preparation method of low alkali value BIT liquid preparation, is comprised the following steps that：
(1) BIT 25.0wt%, propane diols 50.0wt%, bay are weighed respectively as requested
Base sulfanilic acid 0.3wt%, ethylenediamine tetra-acetic acid 0.8wt%, deionized water 27.8wt%；
(2) load weighted propane diols, lauryl sulfonic acid amine are sequentially added in four mouthfuls of reactors, is stirred under 150rpm rotating speed
Mix, and then warming-in-water adds BIT to 40-50 DEG C, continue 150rpm and be dispersed with stirring 30min；
(3) ethylenediamine tetra-acetic acid is equably added dropwise in the reactor of step (2), time for adding is 0.5 hour, reaction
Temperature is at 55-60 DEG C, after being added dropwise to complete, stirring reaction 5 hours；
(4) add deionized water to continue after reacting 1 hour, be down to room temperature, obtain low alkali value 1,2- benzisothiazoles -3-
Ketone liquid preparation.
The low alkali value BIT liquid preparation is weak yellow liquid, and pH is 7.0~8.5.
Embodiment 4
A kind of preparation method of low alkali value BIT liquid preparation, is comprised the following steps that：
(1) BIT 28.0wt%, dipropylene glycol are weighed respectively as requested
50.0wt%, acesulfame potassium 0.5wt%, phytic acid 0.7wt%, deionized water 28.2wt%；
(2) load weighted dipropylene glycol, acesulfame potassium are sequentially added in four mouthfuls of reactors, in turning for 150rpm
Speed is lower to be stirred, and then warming-in-water adds BIT to 40-50 DEG C, continue 150rpm and be dispersed with stirring
30min；
(3) phytic acid is equably added dropwise in the reactor of step (2), time for adding is 0.5 hour, and reaction temperature exists
55-60 DEG C, after being added dropwise to complete, stirring reaction 5 hours；
(4) add deionized water to continue after reacting 1 hour, be down to room temperature, obtain low alkali value 1,2- benzisothiazoles -3-
Ketone liquid preparation.
The low alkali value BIT liquid preparation is weak yellow liquid, and pH is：7.0~8.5.
Embodiment 5
A kind of preparation method of low alkali value BIT liquid preparation, is comprised the following steps that：
(1) BIT 30.0wt%, dipropylene glycol are weighed respectively as requested
60.0wt%, acesulfame potassium 1.2wt%, phytic acid 1.2wt%, deionized water 30.0wt%；
(2) load weighted dipropylene glycol, acesulfame potassium are sequentially added in four mouthfuls of reactors, in turning for 150rpm
Speed is lower to be stirred, and then warming-in-water adds BIT to 40-50 DEG C, continue 150rpm and be dispersed with stirring
30min；
(3) phytic acid is equably added dropwise in the reactor of step (2), time for adding is 0.5 hour, and reaction temperature exists
55-60 DEG C, after being added dropwise to complete, stirring reaction 5 hours；
(4) add deionized water to continue after reacting 1 hour, be down to room temperature, obtain low alkali value 1,2- benzisothiazoles -3-
Ketone liquid preparation.
The low alkali value BIT liquid preparation is weak yellow liquid, and pH is 7.0~8.5.
Low alkali value 1,2- benzisothiazole-3-ketones liquid preparation obtained by upper 5 groups of embodiments is subjected to quality inspection
Survey.See Fig. 3, Fig. 4 compared with the BIT (control group) of three producers of market purchasing, the present invention
The low alkali value BIT liquid preparation of made moral has bactericidal activity high, alkaline low, good water solubility, resists
Low temperature, good dispersion, low cost and other advantages.
Claims (9)
1. a kind of low alkali value BIT liquid preparation, it is characterised in that by the component of following weight proportion
Composition：BIT 15.0wt%~30.0wt%, soluble carrier 30.0wt%~60.0wt%, parent
Core reagent 0.2wt%~1.2wt%, catalyst 0.5wt~1.2wt%, deionized water 20.0wt%~30.0wt%.
A kind of 2. low alkali value BIT liquid preparation according to claim 1, it is characterised in that
The soluble carrier is polyalcohol or polyol derivative.
A kind of 3. low alkali value BIT liquid preparation according to claim 1, it is characterised in that
The nucleopilic reagent is sulfonate.
A kind of 4. low alkali value BIT liquid preparation according to claim 3, it is characterised in that
The sulfonate is lauryl sulfonic acid amine, a- olefin sulfonic acids amine or acesulfame potassium.
A kind of 5. low alkali value BIT liquid preparation according to claim 1, it is characterised in that
The catalyst is carboxylic acids catalyst.
A kind of 6. low alkali value BIT liquid preparation according to claim 5, it is characterised in that
The carboxylic acids catalyst is citric acid, ethylenediamine tetra-acetic acid, phytic acid and/or gluconic acid.
A kind of 7. low alkali value BIT liquid preparation according to claim 1, it is characterised in that
The deionized water resistivity is more than 0.5M Ω cm.
A kind of 8. low alkali value BIT liquid preparation according to claim 1, it is characterised in that
The low alkali value BIT liquid preparation is weak yellow liquid, and pH is 7.0~8.5.
9. a kind of preparation method of low alkali value BIT liquid preparation as claimed in claim 1, it is special
Sign is to comprise the following steps that：
(1) weigh respectively as requested 1,2- benzisothiazole-3-ketones, nucleopilic reagent, soluble carrier, catalyst, go from
Sub- water；
(2) load weighted soluble carrier, nucleopilic reagent are sequentially added in four mouthfuls of reactors, are stirred under 150rpm rotating speed,
And then warming-in-water adds BIT to 40-50 DEG C, continue 150rpm and be dispersed with stirring 30min；
(3) catalyst is equably added dropwise in the reactor of step (2), time for adding is 0.5 hour, and reaction temperature is in 55-
60 DEG C, after being added dropwise to complete, stirring reaction 5 hours；
(4) add deionized water to continue after reacting 1 hour, be down to room temperature, obtain low alkali value BIT liquid
Body preparation.
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| CN201711192056.1A CN107821405A (en) | 2017-11-24 | 2017-11-24 | A kind of ketone liquid preparation of 1,2 benzisothiazole of low alkali value 3 and preparation method |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103619174A (en) * | 2011-05-13 | 2014-03-05 | Isp投资公司 | Aqueous solutions of 1,2-benzisothiazolin-3-one |
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- 2017-11-24 CN CN201711192056.1A patent/CN107821405A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103619174A (en) * | 2011-05-13 | 2014-03-05 | Isp投资公司 | Aqueous solutions of 1,2-benzisothiazolin-3-one |
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Application publication date: 20180323 |