CN102920617A - Liquid type deet composition and preparation thereof - Google Patents

Liquid type deet composition and preparation thereof Download PDF

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Publication number
CN102920617A
CN102920617A CN2012104595905A CN201210459590A CN102920617A CN 102920617 A CN102920617 A CN 102920617A CN 2012104595905 A CN2012104595905 A CN 2012104595905A CN 201210459590 A CN201210459590 A CN 201210459590A CN 102920617 A CN102920617 A CN 102920617A
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diethyltoluamide
compositions
water
aqua type
water aqua
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CN102920617B (en
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郑庆康
许晓锋
郑进渠
雷乐颜
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Sichuan University
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Sichuan University
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Abstract

The invention discloses a liquid type deet composition and a preparation method of the composition. The composition comprises the following main ingredients: water, deet, fatty alcohol polyoxyethylene ether sodium sulfate, triethanolammonium dodecylbenzene sulfonate, a nonionic surfactant and a cationic surfactant, and is prepared by adding the surfactant into deet, mixing and slowing adding water, and naturally emulsifying. The preparation method is simple in process, low in cost, environment-friendly; the composition has a mosquito repelling function.

Description

A kind of water aqua type diethyltoluamide compositions and preparation thereof
Technical field
The invention belongs to the detergents and cosmetic field, be specifically related to a kind of anophelifuge composition and method of making the same.
Background technology
Diethyltoluamide (DEET) was developed by the U.S. in 1956, because it has the insect repellant effect of wide spectrum and good repellent effect worldwide is widely used.Yet diethyltoluamide crude oil the shortcoming such as generally has and abnormal smells from the patient is bad greasy, scorching hot in smearing the skin process, even the anaphylaxiss such as erythema, decortication can occur, so need to be processed into different application state (dosage form) in order to use safety.
The anophelifuge application forms can be divided three classes by different phase.The first kind is solid kind, with mosqito repellent absorption wherein, comprises the dosage forms such as anophelifuge powder, anophelifuge paper, mosquito-dispelling tablet take solid as carrier.Such as publication number be CN88105401A patent disclosure make the method for anophelifuge powder as substrate absorption anophelifuge as carrier, starch take molecular sieve or clay material.Although this type of material can obtain preferably repelling effect, be not suitable for skin and smear.Equations of The Second Kind is the aerosol class, is filled with noble gas mosqito repellent is treated to the aerosol state.Such as publication number be CN102396572A patent disclosure make the method for aerosol mosquito repelling agent with diethyltoluamide 10-20%, citronella oil 10-20%, Polyethylene Glycol 10-20%, noble gas 50-80%.This type of material is easy to use, and is satisfactory for result, but cost is higher.The 3rd class is liquid type, and this type of is most widely used, utilizes ethanol, aromatic hydrocarbons, water equal solvent dissolving mosqito repellent to make stabilizing solution, comprises the dosage forms such as mosquito-repellent perfume, mosquito-dispelling cream, anophelifuge breast and mosquito-driving liquid.At present most solutions class anophelifuge product uses ethanol to be solvent, i.e. tincture, such as publication number be CN1019140539A and CN1334005A patent disclosure all prepare mosquito-driving liquid take the ethanol of 10-40% as solvent.Diethyltoluamide is dissolved in the ethanol, although have preferably mosquito-proof and sterilizing function, because ethanol has suitable defat and volatility, can make the normal cutin solution-off of skin and skin surface dehydration.In addition, anophelifuge solution can also be made oil-type and smear mosquito-proofly, be that CN1391800A discloses the method for using zinc stearate, magnesium stearate, glycerol, Polyethylene Glycol and water to make a kind of anophelifuge such as publication number.Summer, heat was easily sweat, and used this product more can make us feeling much depressed, and lacked clearly sense and not easy cleaning.
Water aqua type anophelifuge solution, namely with surfactant with in the diethyltoluamide dissolved water.The advantage of using this dosage form is easy cleaning, feels comfortable, does not have organic solvent to the harmful effect of skin.But because diethyltoluamide is oily matter, be difficult in the dissolved water, cause whole solution system more unstable.Publication number be CN101073538A patent disclosure a kind of mosquito repellent composition make the water aqua type emulsion by emulsifying agent, anophelifuge and moisturizing agent, utilize but be not easy to dilution, and added antiseptic.
Diethyltoluamide also has the uvioresistant effect except anti-mosquito function.The people such as beam Jingjing deliver " research of aromatic polyamide fabric anti-ultraviolet ageing " and find greatly to increase through the kevlar fabric uvioresistant performance that diethyltoluamide is processed at " synthetic fibers ", the strength retention of fabric reaches 87 % behind 100 h ultraviolet ageings, far surpasses strength retention 42 % after unprocessed fabric wears out.Diethyltoluamide is prepared into the anti UV finishing that water aqua type solution can also make things convenient for fabric to carry out.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of water aqua type compositions of diethyltoluamide, with an organic solvent to overcome product to stimulation and the infringement of skin, does not possess higher solution-stabilized performance in order to use in wider concentration range, thereby effectively mosquito-proof.
In order to solve the problems of the technologies described above, the invention provides a kind of water aqua type compositions of diethyltoluamide, by active component and water by mass percentage 1-50 % mix and make.The content mass percent of the active component of described compositions is as shown in table 1.
Active component and the content of table 1 water aqua type diethyltoluamide compositions
Figure 301427DEST_PATH_IMAGE002
Wherein, described non-ionic surface active agent is polystyrene phenol polyoxyethylene ether, C 8-9Alkylphenol-polyethenoxy-4-ether, Zhong Xin phenol polyethenoxy-10-ether, C 12In aliphatic alcohol polyethenoxy-7-ether one or several.
Described cationic surfactant is one or several in octadecylamine polyoxyethylene ether bi-quaternary ammonium salt, two lauryl amine polyoxyethylene ether mono-quaternaries, the dodecyl dimethyl benzyl ammonium chloride.
The present invention also provides a kind of preparation method of above-mentioned water aqua type diethyltoluamide compositions, and described preparation method comprises the steps:
Content by the mass percent of the composition of the water aqua type compositions of above-mentioned diethyltoluamide is put into agitator tank successively with the component of each effective ingredient, stirs 5-10 min in temperature is 20-30 ℃ of scope; Slowly add entry and make certain proportion (effective ingredient mixes with water for 1-50% by mass percentage) solution, continue to stir 10-20 min in 30-60 ℃ of scope, cooling is left standstill.
The present invention forms micelle parcel diethyltoluamide in aqueous solution by compound surfactant, and it is less to have obtained the emulsifying microgranule, the water aqua type solution system that stability is high.
The present invention also provides the purposes of a kind of above-mentioned water aqua type diethyltoluamide compositions aspect anophelifuge.
Advantage of the present invention is: the first, and technique is made simple, and configuration is convenient, and is with low cost; The second, not with an organic solvent and antiseptic, reduce stimulation and infringement to skin, the environmental protection low toxicity; The 3rd, the product of preparation has good solution stability, and the concentration range of use is wider, can be mixed with water in effective ingredient is 1-50% concentration (mass percent) scope.
The specific embodiment
Explain the present invention below in conjunction with embodiment.Embodiment is for ease of better understanding the present invention, but is not limitation of the present invention.
Embodiment 1:
A kind of water aqua type diethyltoluamide compositions, by active component with the 5%(mass percent) mix with water and to make, wherein active component is to mix and get in each component content ratio of table 2.
Active component and the content of the water aqua type diethyltoluamide compositions of table 2 embodiment 1
Figure 653911DEST_PATH_IMAGE003
The preparation method of the water aqua type diethyltoluamide compositions of embodiment 1: successively diethyltoluamide, farming breast 600, AES, DBSA triethanolamine salt are put into agitator tank by the aforementioned proportion in the table 2, in being 20-30 ℃ of scope, temperature stirs 5-10 min, slowly adding entry, to make active component be the 5%(mass percent) solution, 10-20 min is stirred in continuation in 30-60 ℃ of scope, cooling is left standstill and obtained water aqua type diethyltoluamide compositions.Prepared product safety is nontoxic, and anophelifuge effective time reaches 8 hours.
Embodiment 2:
A kind of water aqua type diethyltoluamide compositions, by active component with the 10%(mass percent) mix with water and to make, wherein active component is to mix and get in each component content ratio of table 3.
Active component and the content of the water aqua type diethyltoluamide compositions of table 3 embodiment 2
Figure 661706DEST_PATH_IMAGE004
The preparation method of the water aqua type diethyltoluamide compositions of embodiment 2: successively diethyltoluamide, OP-4, OP-10, AES, DBSA triethanolamine salt are put into agitator tank by the aforementioned proportion in the table 3, in being 20-30 ℃ of scope, temperature stirs 5-10 min, slowly adding entry, to make active component be the 10%(mass percent) solution, 10-20 min is stirred in continuation in 30-60 ℃ of scope, cooling is left standstill and obtained water aqua type diethyltoluamide compositions.The product safety that makes is nontoxic, and anophelifuge effective time reaches 12 hours.
Embodiment 3:
A kind of water aqua type diethyltoluamide compositions, by active component with the 20%(mass percent) mix with water and to make, wherein active component is to mix and get in each component content ratio of table 4.
Active component and the content of the dosage form diethyltoluamide compositions of table 4 embodiment 3
Figure 99641DEST_PATH_IMAGE005
The preparation method of the water aqua type diethyltoluamide compositions of embodiment 3: successively diethyltoluamide, OP-4, AEO-7, AES, octadecylamine polyoxyethylene ether bi-quaternary ammonium salt are put into agitator tank by the aforementioned proportion in the table 4, in being 20-30 ℃ of scope, temperature stirs 5-10 min, slowly adding entry, to make active component be the 20%(mass percent) solution, 10-20 min is stirred in continuation in 30-60 ℃ of scope, cooling is left standstill and obtained water aqua type diethyltoluamide compositions.The product safety that makes is nontoxic, and anophelifuge effective time reaches 17 hours.
Embodiment 4:
A kind of water aqua type diethyltoluamide compositions, by active component with the 10%(mass percent) mix with water and to make, wherein active component is to mix and get in each component content ratio of table 5.
Active component and the content of the dosage form diethyltoluamide compositions of table 5 embodiment 4
The preparation method of the water aqua type diethyltoluamide compositions of embodiment 4: successively diethyltoluamide, OP-4, AEO-7, AES, two lauryl amine polyoxyethylene ether mono-quaternaries are put into agitator tank by the aforementioned proportion in the table 5, in being 20-30 ℃ of scope, temperature stirs 5-10 min, slowly adding entry, to make active component be the 10%(mass percent) solution, 10-20 min is stirred in continuation in 30-60 ℃ of scope, cooling is left standstill and obtained water aqua type diethyltoluamide compositions.The product safety that makes is nontoxic, and anophelifuge effective time reaches 13 hours.
Embodiment 5:
(1) evaluating drug effect test.
Detect foundation: according to the pertinent regulations of GB GB/T 17322.10-1998, carry out human trial and drug effect is made evaluation.
For trying insecticide: Aedes albopictus (Aedes albopictus), the normal strain of indoor feeding, the female insect of not sucking blood in 4-5 days after sprouting wings.
Detection method: before the experiment testing crew and used examination worm are carried out the attack test: the back of the hand exposes 4 cm * 4 cm skins, and remainder tightly covers.In the mosquito cage of long 40 cm * wide 30 cm * high 30 cm, put into 300 examination worms; after mosquito recovers normal activity; hands is stretched into placement 2 min in the mosquito cage, and the examination worm that comes to stop falling is qualified for attack more than 30 persons, and this person and this cage mosquito can be used for repellency test.Select qualified examination worm and 3 experimenters of attack, respectively draw the skin area of 5 cm * 5 cm at people's both hands back, wherein a hands is blank, and the another hands is by 1.5 μ l/cm 2Dosage evenly smear repellant to be measured, expose wherein 4 cm * 4 cm skins, tightly cover remainder.Smear 2 h after the repellant, hands is stretched into 2 min in the cage that is placed with the qualified mosquito of attack.Observation has or not mosquito to come to suck blood, and per hour test is once made repellant and lost efficacy as long as have 1 mosquito to come to suck blood namely to declare later on.The effective protecting time (h) of record repellant.Result of the test is as shown in table 6 below.
The effect experiment result of the water aqua type diethyltoluamide compositions that table 6 embodiment 1-4 prepares
Figure 55144DEST_PATH_IMAGE007
Result of the test shows: the water aqua type diethyltoluamide compositions repelling effect of embodiment 1-4 is remarkable, is 7-18 h to the effective protecting time of human body, and indoor harmacological effect all reaches national standard A level.
(2) toxicological test.
Detect foundation: according to GB GB15670-1995 pertinent regulations, carry out toxicological test and to skin irritation reaction make evaluation.
For trying animal: 4 of one-level new zealand rabbits, body weight 2.5-2.9 Kg is provided by Sichuan University's Experimental Animal Center.
Detection method: test and rabbit driven back spinal column both sides cropping in front 24 hours, area respectively is 2 * 3 cm 2After 24 hours, inspection skin is got tested material stock solution 0.5 ml without breakage, is coated on the animal subject one side cropping skin, and the oilpaper gauze covers, and rubber plaster is fixed, take opposite side skin as contrast, and the coating normal saline.The coating tested material dismantled after 4 hours, cleaned residual tested material with clear water, and after 1,2,3 day, whether local skin has erythema, edema to form after the observed and recorded cleaning tested material, by the scoring of skin irritation reaction standards of grading.Result of the test is as shown in table 7 below.
The toxicological experiment result of the water aqua type diethyltoluamide compositions that table 7 embodiment 1-4 prepares
Figure 168594DEST_PATH_IMAGE008
Result of the test shows: the water aqua type diethyltoluamide compositions anophelifuge of embodiment 1-4 all belongs to nonirritant to the stimulus intensity of rabbit.

Claims (6)

1. a water aqua type diethyltoluamide compositions is characterized in that, the composition of the active component of described compositions and content mass percent thereof are:
Diethyltoluamide: 60-85%
Polyoxyethylenated alcohol sodium sulfate: 1-10%
DBSA triethanolamine salt: 0-8%
Cationic surfactant: 0-5%
Non-ionic surface active agent: 10-20%
Effective ingredient by mass percentage 1-50 % mixes with water.
?
2. water aqua type diethyltoluamide compositions as claimed in claim 1 is characterized in that, the composition of the active component of described compositions and preferred content mass percent thereof are:
Diethyltoluamide: 78-80%
Polyoxyethylenated alcohol sodium sulfate: 2-5%
DBSA triethanolamine salt: 0-4%
Cationic surfactant: 0-2%
Non-ionic surface active agent: 14-18%
Effective ingredient by mass percentage 1-50 % mixes with water.
?
3. water aqua type diethyltoluamide compositions as claimed in claim 1 or 2 is characterized in that, described non-ionic surface active agent is polystyrene phenol polyoxyethylene ether, C 8-9Alkylphenol-polyethenoxy-4-ether, Zhong Xin phenol polyethenoxy-10-ether, C 12In aliphatic alcohol polyethenoxy-7-ether one or several.
?
4. water aqua type diethyltoluamide compositions as claimed in claim 1 or 2, it is characterized in that described cationic surfactant is one or several in octadecylamine polyoxyethylene ether bi-quaternary ammonium salt, two lauryl amine polyoxyethylene ether mono-quaternaries, the dodecyl dimethyl benzyl ammonium chloride.
?
5. the preparation method of water aqua type diethyltoluamide compositions as claimed in claim 1 or 2 is characterized in that described method comprises the steps:
Component and content by claim 1 or 2 described each effective ingredient are put into agitator tank successively, in being 20-30 ℃ of scope, temperature stirs 5-10 min, slowly add entry and make certain proportion solution, continue to stir 10-20 min in 30-60 ℃ of scope, cooling is left standstill; Wherein certain proportion refer to described effective ingredient by mass percentage 1-50 % mix with water.
?
6. claim 1 or the purposes of 2 described water aqua type diethyltoluamide compositionss aspect anophelifuge.
CN201210459590.5A 2012-11-15 2012-11-15 Liquid type deet composition and preparation thereof Expired - Fee Related CN102920617B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS52110824A (en) * 1976-03-16 1977-09-17 Tsumura Juntendo Kk Insect preventive agent
JPS58198403A (en) * 1982-05-14 1983-11-18 Nippon Oil & Fats Co Ltd Insect repellent composition
CN1094087A (en) * 1993-04-08 1994-10-26 科尔加特·帕尔莫利弗公司 The household liquids detergent composition that contains wormer
JP2001048713A (en) * 1999-08-02 2001-02-20 Earth Chem Corp Ltd Stabilization of tralomethrin aqueous solution

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS52110824A (en) * 1976-03-16 1977-09-17 Tsumura Juntendo Kk Insect preventive agent
JPS58198403A (en) * 1982-05-14 1983-11-18 Nippon Oil & Fats Co Ltd Insect repellent composition
CN1094087A (en) * 1993-04-08 1994-10-26 科尔加特·帕尔莫利弗公司 The household liquids detergent composition that contains wormer
JP2001048713A (en) * 1999-08-02 2001-02-20 Earth Chem Corp Ltd Stabilization of tralomethrin aqueous solution

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
谢敬松等: "驱蚊霜避蚊效果观察", 《中华卫生杀虫药械》, vol. 9, no. 2, 31 December 2003 (2003-12-31), pages 70 - 72 *

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