CN106538517B - Abietyl pesticide solvent and preparation method thereof - Google Patents

Abietyl pesticide solvent and preparation method thereof Download PDF

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CN106538517B
CN106538517B CN201610976729.1A CN201610976729A CN106538517B CN 106538517 B CN106538517 B CN 106538517B CN 201610976729 A CN201610976729 A CN 201610976729A CN 106538517 B CN106538517 B CN 106538517B
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rosin
preparation
abietyl
basic catalyst
mixture
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CN106538517A (en
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张玲钰
赵庆平
杨航周
黄启朋
孔雷
李修刚
卢筱筱
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Huizhou Yinnong Technology Co ltd
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Tongren University
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/02Biocides, 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)
  • Toxicology (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Agronomy & Crop Science (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Fats And Perfumes (AREA)

Abstract

The present invention provides a kind of abietyl pesticide solvent and preparation method thereof, is related to pesticide solvent field.The preparation method includes: to mix rosin, waste oil, the first basic catalyst and glycerol, and under vacuum condition, heating, esterification obtains the first mixture that acid value is less than 1mgKOH/g;Low-carbon alcohols are added in the first mixture, filter out the first basic catalyst, are added the second basic catalyst, the ester exchange reaction 3h-5h under the conditions of 60 DEG C -80 DEG C obtains the second mixture, cooling layering, and ester layer is decolourized dealcoholysis, abietyl pesticide solvent is obtained;Wherein, the mass ratio of rosin and waste oil is 3-7:3-7;1-1.5 times of the integral molar quantity of the inventory rosin acid and fatty acid of glycerol;The preparation method production cost is low, and product yield is high.The abietyl pesticide solvent raw material sources are extensive, safety and stability, are worth with certain business promotion.

Description

Abietyl pesticide solvent and preparation method thereof
Technical field
The present invention relates to a kind of pesticide solvent fields, and in particular to a kind of abietyl pesticide solvent and preparation method thereof.
Background technique
Since the eighties in last century, because producing, storing and transporting safety and health, the risk of environment, the developed countries such as America and Europe Prohibit successively in pesticide, limited the use of light aromatic solvent, missible oil solvent is gradually substituted by safer solvent.And in China, Missible oil dosage form still accounts for the 50% of current pesticidal preparations usage amount, and about 1,000,000 tons, average year consumes more than 30 ten thousand tons of light aromatic solvents, Thus bring safety, environment and health problem can not be ignored.For this purpose, country has put into effect some policies and regulations limitation creams in recent years The production and use of oil, and waterborne preparation and non-aromatic alkyl are guided and helped energetically by estate planning, science and technology item etc. The development of missible oil.
On long terms, cream preparation is because having many advantages, such as simple production process, preparation stabilization, easy to use, good drug efficacy, still It will be one of main dosage form of pesticide, even if still having 25% or more market in the American-European countries of waterborne preparation high development Share.Thus, solve the problems, such as that the fundamental way of missible oil necessarily finds the safety and environmental protection substitute of light aromatic solvent, to complete The green upgrading of traditional missible oil.The substitute of optimal conventional solvent is vegetable oil solvent currently on the market, wherein Fujian promise The turpentine-based vegetable oil that moral Biotechnology Co., Ltd prepares using rosin and vegetable oil as raw material is due to solubility and safety ratio It is more satisfactory, the approval in market is gradually obtained, and applied for a kind of agricultural combination solvent of patent of invention CN102524246A and its answered With, CN101984806A contain terpene vegetable oil composition and its application, a kind of turpentine-based vegetable oil of CN101984805A and Preparation method and application.However there is following problems for the method: 1, using rosin as raw material, causing high value in rosin The terebinthine waste of product;2, using vegetable oil as raw material, the problem of there is " striving food with the people ";3, pass through high shear and ultrasound cream Chemical industry skill mixes the carboxylate of rosin and grease, is long placed in the risk in the presence of layering.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of abietyl pesticide solvent, safety and stability is made, to ring The beneficial abietyl pesticide solvent in border, this method production cost is low, and product yield is high.
Another object of the present invention is to provide a kind of abietyl pesticide solvents, are made by above-mentioned preparation method, the pine The raw material sources of perfume base pesticide solvent are extensive, safety and stability, are a kind of environment friendly agricultural solvents to environmental beneficial, have centainly Business promotion value.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes a kind of preparation method of abietyl pesticide solvent comprising:
Rosin, waste oil, the first basic catalyst and glycerol are mixed, under vacuum condition, heating, esterification is obtained Acid value is less than the first mixture of 1mgKOH/g;Low-carbon alcohols are added in first mixture, filter out the first basic catalyst, are added the Two basic catalysts, the ester exchange reaction 3h-5h under the conditions of 60 DEG C -80 DEG C obtain the second mixture, and cooling layering takes off ester layer Color dealcoholysis obtains abietyl pesticide solvent.
Wherein, the mass ratio of rosin and waste oil is 3-7:3-7;The inventory of glycerol is the rosin acid that rosin contains and gives up 1-1.5 times of the integral molar quantity for the fatty acid that grease contains.
The abietyl pesticide solvent as made from above-mentioned preparation method, it is good with pesticide compatibility, and safety and stability, have to environment Benefit is a kind of environment friendly agricultural solvent.
The beneficial effect of abietyl pesticide solvent provided in an embodiment of the present invention and preparation method thereof is: this method is using pine Remaining cheap rosin is raw material after rouge removes turpentine oil, avoids terebinthine waste;With swill oil, gutter oil, acidification oil And the waste greases such as useless animal fat are raw material, while the problem of not only avoiding " striving food with the people ", go back changing waste into valuable, subtract Few a large amount of waste greases are used for food processing by illegal retailer, ensure society and food safety;Pass through prolonged high temperature esterification Reaction and ester exchange reaction are, it can be achieved that rosin acid low carbon alcohol ester and fatty acid ester of low-carbon alcohol are thoroughly mixed, safety and stability.Pass through The total recovery of abietyl pesticide solvent made from above-mentioned preparation method can reach 90% or more, and production cost can reduce by 29%.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the flow chart for the preparation method that the embodiment of the present invention 1 provides;
Fig. 2 is the flow chart for the preparation method that the embodiment of the present invention 5 provides.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase Product.
Abietyl pesticide solvent of the embodiment of the present invention and preparation method thereof is specifically described below.
The preparation method of abietyl pesticide solvent, comprising:
Rosin, waste oil, the first basic catalyst and glycerol are mixed, under vacuum condition, heating, esterification is obtained Acid value is less than the first mixture of 1mgKOH/g.
Wherein, rosin refers to the non-volatile natural tree using pine resin as raw material, obtained by different processing methods The main component of rouge, rosin is rosin acid, is a kind of tricyclic diterpene class oxygenatedchemicals, not soluble in water, is dissolved in general organic molten Agent and diluted sodium hydroxide solution are dissolved in alcohol, benzene, chloroform, acetone, ether and carbon disulfide.
Waste oil at least one of is selected from as swill oil, gutter oil, acidification oil and useless animal fat, for example, swill oil or Gutter oil or acidification oil and the mixture of useless animal fat etc., main component are fatty acid.Preferably, waste oil can be with It is pre-processed using preceding, such as is filtered, for removing the impurity in waste oil, while can also will be obtained after filtering Waste oil carry out heating concentration, to improve the content of grease in waste oil.
Preferably, the mass ratio of rosin and waste oil is 3-7:3-7, and within the scope of this, finally formed abietyl pesticide is molten The compatibility performance of agent and pesticide activity component is more excellent.
Glycerol also known as glycerine are colourless sweet clear and bright thick liquid, can be arbitrarily miscible with water, ethyl alcohol.Preferably, sweet The inventory of oil is 1-1.5 times of the integral molar quantity for the fatty acid that the rosin acid that rosin contains and waste oil contain, to make pine The fatty acid that the rosin acid and waste oil that perfume (or spice) contains contain sufficiently is reacted with glycerol, is not wasted raw material.
First basic catalyst is used to be catalyzed the esterification for accelerating rosin, waste oil and glycerol, it is preferable that the first alkalinity Catalyst is MOH/NxOyType solid base, wherein MOH is alkali metal hydroxide, NxOyFor carrier, catalytic activity is high, favorably In the abundant progress for promoting esterification.Specifically, MOH/NxOyType solid base can be selected from NaOH/SiO2、NaOH/γ- Al2O3、NaOH/TiO2、KOH/SiO2、KOH/γ-Al2O3And KOH/TiO2At least one of, such as MOH/NxOyType solid base For NaOH/ γ-Al2O3Or NaOH/TiO2Or MOH/NxOyType solid base is NaOH/ γ-Al2O3、NaOH/TiO2And KOH/SiO2 Mixture.First basic catalyst can be preferably powdered to be blocky or powdered, to increase it between catalysant Contact area, improve catalytic efficiency.
Preferably, the inventory of the first basic catalyst accounts for the 0.1%-2% of the total amount of feeding of rosin and waste oil, the model In enclosing, catalytic efficiency is best, and rosin, waste oil is made not to waste the first catalyst while sufficiently reaction with glycerol, saves production Cost.It is noted that the first basic catalyst it is repeatable be recycled it is multiple, it is preferable that the first basic catalyst is to multiple It uses 3 times again, it is highly preferred that the first basic catalyst is reused 3 times, to realize on the basis of catalytic effect is good further Save the purpose of cost of manufacture.
Specifically, vacuum condition refers to that vacuum degree is lower than the environment of 0.095Mpa, preferably, vacuum degree control is existed 0.085Mpa-0.095Mpa is advisable.Heating and temperature control is 180 DEG C -260 DEG C, and under this condition, esterification can faster reach Chemical balance, effect are best.Preferably, can be constantly stirred in heating process, make it is heated more evenly, each effective component it Between contact also more sufficiently.Preferably, under the above conditions, which carries out 3h-6h, so that reaction obtains acid value and is less than The first mixture of 1mgKOH/g, the first mixture main active are rosin triglyceride and fatty glyceride.
Acid value described herein is also known as neutralization number, acid value, acidity, is to free carboxylic acid groups number in compound or mixture One measurement criteria of amount, in this preparation method, acid value can be measured by national standard " GB/T5530-1985 ".
Low-carbon alcohols are added into the first mixture, filter out the first basic catalyst, the second basic catalyst are added, in 60- Ester exchange reaction 3-5 hours under the conditions of 80 DEG C, the second mixture is obtained.
Wherein, low-carbon alcohols are for diluting the first mixture and as reaction raw materials, it is preferable that low-carbon alcohols are to contain 1-4 At least one of the alcohol of a carbon atom, such as methanol, ethyl alcohol, isopropanol, n-butanol or methanol and the mixture of ethyl alcohol etc.;More Preferably, low-carbon alcohols are at least one of methanol and ethyl alcohol, cheap, reduction cost of manufacture.Low-carbon alcohols are added, may be used also To reduce the amount of above-mentioned first mixture of the first basic catalyst surface filtered out attachment.
Second basic catalyst is preferably at least one of LiOH, NaOH and KOH, such as LiOH or NaOH and KOH Mixture etc., alkalinity are better than the first basic catalyst, keep ester exchange reaction more abundant.
The inventory of second basic catalyst is the 0.7%-1.5% of the total amount of feeding of rosin and waste oil, within the scope of this, Catalytic efficiency is best, it is made not waste the second catalyst while sufficiently reaction, saves cost of manufacture.Second basic catalyst can Think blocky, powdered, since it is dissolved in reaction system, state influences little.It is not limited here.
Carry out ester exchange reaction 3h-5h under the conditions of 60 DEG C -80 DEG C, ester exchange reaction be mainly fatty glyceride with it is low Carbon alcohol generates fatty acid ester of low-carbon alcohol and glycerol under the catalysis of the second basic catalyst, and rosin triglyceride and low-carbon alcohols are New rosin acid low carbon alcohol ester and glycerol are generated under the catalysis of two basic catalysts, make second by prolonged ester exchange reaction Fatty acid ester of low-carbon alcohol and rosin acid low carbon alcohol ester in mixture reach balance, the rosin acid for being thoroughly mixed it, and obtaining Compatibility is good between ester of low-carbon alcohol and fatty acid ester of low-carbon alcohol, therefore the drawbacks of being long placed in layering is not present in the two, to improve it Holding time.
By the second mixture cool down be layered, due to carboxylate insoluble in glycerol and density ratio glycerol it is small, so upper layer be ester Layer, lower layer is glycerin layer, and ester layer is decolourized dealcoholysis, abietyl pesticide solvent is obtained.
Preferably, ester layer is decolourized using decolorising agent, dealcoholysis is carried out by the way of distillation, improved final obtained The purity of abietyl pesticide solvent.It is finally obtained it is faint yellow to light brown transparent oil be abietyl pesticide solvent.Its Main ingredient is fatty acid ester of low-carbon alcohol and rosin acid low carbon alcohol ester, has good compatibility performance with pesticide activity component, and With good frost resistance, permeability, anti-drift film forming and emulsifying dispersivity are opened up, is a kind of functional agriculture of function admirable Drug carrier has superior materialization and biological property compared with the aromatic hydrocarbons organic solvent such as dimethylbenzene, therefore is preparing pesticide The aromatic hydrocarbons organic solvents such as dimethylbenzene are substituted when preparation.The preparation method flow chart of abietyl pesticide solvent provided above please join Fig. 2 is read, and specific practical manner please refers to embodiment 5.
Preferably, the glycerol after reaction can also be recycled, such as be operated as follows: cooled down to reaction system After layering, glycerin layer acid is taken to neutralize, and filter react salt be precipitated after be evaporated under reduced pressure, recycling obtains glycerol and carries out circulation making With to reduce cost of manufacture.Comprising the process flow recycled to the glycerol after reaction, referring to Fig. 1, and specific practical behaviour Embodiment 1 is please referred to as mode.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
Powdered NaOH/Al by the waste oil of 50kg and 50kg rosin, with rosin and the total input amount 1% of waste oil2O3Type 1.2 times of the integral molar quantity for the fatty acid that the rosin acid and waste oil that solid base catalyst (1kg) and rosin contain contain Glycerol mixing, under conditions of vacuum degree 0.085-0.095Mpa, is stirred and heated to 180 DEG C, esterification 6h obtains acid value The first mixture of 0.3mgKOH/g.After methanol dilution is added in above-mentioned first mixture, NaOH/Al is filtered out2O3Type solid base is urged Agent adds 1.5% NaOH (1.5kg) of rosin and the total input amount of waste oil, and ester exchange reaction 3h is carried out at 65 DEG C, The second mixture is obtained, this, which after reaction cools down the second mixture, is layered, and upper layer is ester layer, and ester layer is decolourized to obtain after dealcoholysis It is faint yellow to light brown transparent oily liquid be abietyl pesticide solvent.Lower layer's glycerin layer is neutralized through acid, filters off the salt of precipitation After be evaporated under reduced pressure, recycling obtain glycerol.
Embodiment 2
Powdered KOH/Al by the waste oil of 30kg and 70kg rosin, with rosin and the total input amount 1.5% of waste oil2O3 The 1.5 of the integral molar quantity for the fatty acid that the rosin acid and waste oil that type solid base catalyst (1.5kg) and rosin contain contain Glycerol mixing again, under conditions of vacuum degree 0.085-0.095Mpa, is stirred and heated to 230 DEG C, esterification 4h obtains acid The first mixture of valence 0.7mgKOH/g.After methanol dilution is added in above-mentioned first mixture, KOH/Al is filtered out2O3Type solid base Catalyst adds 0.8% NaOH (0.8kg) of rosin and the total input amount of waste oil, ester exchange reaction is carried out at 75 DEG C 5h obtains the second mixture, this, which after reaction cools down the second mixture, is layered, and upper layer is ester layer, after ester layer decoloration dealcoholysis Obtain it is faint yellow to light brown transparent oily liquid be abietyl pesticide solvent.Lower layer's glycerin layer is neutralized through acid, is filtered off and is precipitated Salt after be evaporated under reduced pressure, recycling obtain glycerol.
Embodiment 3
Powdered KOH/Al by the waste oil of 70kg and 30kg rosin, with rosin and the total input amount 0.5% of waste oil2O3 The 1.3 of the integral molar quantity for the fatty acid that the rosin acid and waste oil that type solid base catalyst (0.5kg) and rosin contain contain Glycerol mixing again, under conditions of vacuum degree 0.085-0.095Mpa, agitating and heating obtains acid in 240 DEG C of esterification 5h The first mixture of valence 0.65mgKOH/g.After ethyl alcohol dilution is added in above-mentioned first mixture, KOH/Al is filtered out2O3Type solid base Catalyst adds 0.7% LiOH (0.7kg) of rosin and the total input amount of waste oil, and ester exchange reaction 5h, obtains at 80 DEG C Second mixture, this, which after reaction cools down the second mixture, is layered, and upper layer is ester layer, will obtain after ester layer decoloration dealcoholysis light Yellow to light brown transparent oily liquid is abietyl pesticide solvent, and lower layer's glycerin layer is neutralized through acid, after the salt for filtering off precipitation Vacuum distillation, recycling obtain glycerol.
Embodiment 4
Powdered KOH/TiO by the waste oil of 35kg and 65kg rosin, with rosin and the total input amount 0.1% of waste oil2 The 1.4 of the integral molar quantity for the fatty acid that the rosin acid and waste oil that type solid base catalyst (0.1kg) and rosin contain contain Glycerol mixing again, under conditions of vacuum degree 0.085-0.095Mpa, is stirred and heated to 260 DEG C, esterification 4h obtains acid The first mixture of valence 0.42mgKOH/g.After isopropanol is added in above-mentioned first mixture, KOH/TiO is filtered out2Type solid Base catalyst adds 1.3% NaOH (1.3kg) of rosin and the total input amount of waste oil, the ester exchange reaction 4h at 72 DEG C, The second mixture is obtained, this, which after reaction cools down the second mixture, is layered, and upper layer is ester layer, and ester layer is decolourized to obtain after dealcoholysis Faint yellow to light brown transparent oily liquid is abietyl pesticide solvent, and lower layer's glycerin layer is neutralized through acid, filters off the salt of precipitation After be evaporated under reduced pressure, recycling obtain glycerol.
Embodiment 5
Powdered NaOH/Al by the waste oil of 35kg and 65kg rosin, with rosin and the total input amount 2% of waste oil2O3Type Solid base catalyst and NaOH/TiO2The rosin acid and waste oil that the mixture (2kg) and rosin of type solid base catalyst contain 1 times of glycerol of the integral molar quantity for the fatty acid that rouge contains mixes, and under conditions of vacuum degree 0.085-0.095Mpa, stirring adds Heat obtains the first mixture of acid value 0.56mgKOH/g to 230 DEG C, esterification 3h.Methanol is added in above-mentioned first mixture After dilution, NaOH/Al is filtered out2O3Type solid base catalyst adds 1% NaOH and KOH of rosin and the total input amount of waste oil Mixture (1kg), the ester exchange reaction 3.5h at 60 DEG C obtains the second mixture, this after reaction drops the second mixture Temperature layering, upper layer is ester layer, will ester layer decolourize dealcoholysis after obtain it is faint yellow to light brown transparent oily liquid be abietyl agriculture Medicine solvent.
Comparative example
Embodiment 1-3 is repeated, enough abietyl pesticide solvents are made, Fujian Nuo De Biotechnology Co., Ltd is raw The turpentine-based vegetable oil product of production as a comparison case 1, four are compared, table 1 is obtained.
1 comparing result of table
By 1 gained of table, the appearance of abietyl pesticide solvent made from the present embodiment 1-3 is identical as turpentine-based vegetable oil, To be faint yellow to light brown transparent oily liquid, four density are respectively less than 1, and moisture content is close.But 1-3 of the embodiment of the present invention The fore-running temperature of abietyl pesticide solvent obtained is far longer than the fore-running temperature of turpentine-based vegetable oil, shows in comparative example The high volatility of turpentine-based vegetable oil obtains abietyl pesticide solvent in embodiment, is easy to cause wave by volatilization in use process Take.
The acid value of abietyl pesticide solvent made from 1-3 of the embodiment of the present invention is far smaller than the acid of turpentine-based vegetable oil Value shows that the quality of the fatty acid to dissociate in abietyl pesticide solvent and rosin acid is less than the fat to dissociate in turpentine-based vegetable oil The quality of acid and rosin acid, i.e. its purification degree are higher than turpentine-based vegetable oil.Abietyl pesticide made from 1-3 of the embodiment of the present invention The flash-point (silent) of solvent is above the flash-point (silent) of turpentine-based vegetable oil, further demonstrates that abietyl pesticide solvent volatility It is not easy to catch fire higher than turpentine-based vegetable oil, and compared to turpentine-based vegetable oil, it is safer.1-3 of the embodiment of the present invention is made Abietyl pesticide solvent condensation point it is close with the condensation point of turpentine-based vegetable oil, both show that resistance to frost is suitable.It is comprehensive The premises, the quality of abietyl pesticide solvent produced by the present invention are better than the quality of existing turpentine-based vegetable oil.
Also, the market price of current turpentine-based vegetable oil is 9000 yuan/ton, about 7000 yuan/ton of production cost, and it is sharp The abietyl pesticide solvent produced with this preparation method, production cost can be down to 5000 yuan/ton, and production cost reduces by 29%, And the total recovery of abietyl pesticide solvent can reach 90% or more, have very strong commercial value.
To sum up, the abietyl pesticide solvent and preparation method thereof of the embodiment of the present invention, the preparation method is simple, yield is high, Abietyl pesticide solvent raw material sources obtained are extensive, safety and stability, to environmental beneficial, are a kind of environment friendly agricultural solvents, have Certain business promotion value.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts Every other embodiment, shall fall within the protection scope of the present invention.

Claims (7)

1. a kind of preparation method of abietyl pesticide solvent, characterized in that it comprises:
Rosin, waste oil, the first basic catalyst and glycerol are mixed, are lower than the vacuum condition of 0.095Mpa in vacuum degree Under, 180 DEG C -260 DEG C are heated to, esterification obtains the first mixture that acid value is less than 1mgKOH/g;In first mixture Middle addition low-carbon alcohols filter out first basic catalyst, and the second basic catalyst is added, and ester is handed under the conditions of 60 DEG C -80 DEG C Reaction 3h-5h is changed, obtains the second mixture, ester layer is decolourized dealcoholysis, obtains the abietyl pesticide solvent by cooling layering;
Wherein, the mass ratio of the rosin and the waste oil is 3-7:3-7;The inventory of the glycerol is that the rosin contains Rosin acid and contain 1-1.5 times of the integral molar quantity of fatty acid of the waste oil;
First basic catalyst is MOH/NxOyType solid base, wherein MOH is alkali metal hydroxide, the NxOyTo carry Body, the NxOySelected from SiO2、γ-Al2O3Or TiO2
Second basic catalyst is selected from least one of LiOH, NaOH and KOH;
The low-carbon alcohols are selected from least one of the alcohol containing 1-4 carbon atom;
The waste oil is selected from least one of swill oil, gutter oil, acidification oil and useless animal fat.
2. preparation method according to claim 1, which is characterized in that the MOH/NxOyType solid base is selected from NaOH/ SiO2、NaOH/γ-Al2O3、NaOH/TiO2、KOH/SiO2、KOH/γ-Al2O3And KOH/TiO2At least one of.
3. preparation method according to claim 2, which is characterized in that the inventory of first basic catalyst accounts for described The 0.1%-2% of the total amount of feeding of rosin and the waste oil.
4. preparation method according to claim 1, which is characterized in that the vacuum degree is 0.085Mpa-0.095Mpa.
5. preparation method according to claim 1, which is characterized in that the inventory of second basic catalyst is described The 0.7%-1.5% of the total amount of feeding of rosin and the waste oil.
6. preparation method according to claim 1, which is characterized in that further include being recycled to the glycerol after reaction The step of, the recycling step is to take lower layer to be neutralized with acid after reaction system cooling is layered, and depressurizes steaming after filtering off the salt of precipitation It evaporates, recycling obtains.
7. abietyl pesticide solvent made from preparation method as claimed in any one of claims 1 to 6.
CN201610976729.1A 2016-10-28 2016-10-28 Abietyl pesticide solvent and preparation method thereof Active CN106538517B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101984805A (en) * 2010-07-22 2011-03-16 福建诺德生物科技有限责任公司 Turpentine-based vegetable oil and preparation method and application thereof
CN101984806A (en) * 2010-07-22 2011-03-16 福建诺德生物科技有限责任公司 Terpene-containing vegetable oil composition and applications thereof
CN102524246A (en) * 2010-12-08 2012-07-04 福建诺德生物科技有限责任公司 Agricultural combination solvent and application thereof
CN103224615A (en) * 2013-04-28 2013-07-31 长兴化学工业(广东)有限公司 Alkyd resin composition and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101984805A (en) * 2010-07-22 2011-03-16 福建诺德生物科技有限责任公司 Turpentine-based vegetable oil and preparation method and application thereof
CN101984806A (en) * 2010-07-22 2011-03-16 福建诺德生物科技有限责任公司 Terpene-containing vegetable oil composition and applications thereof
CN102524246A (en) * 2010-12-08 2012-07-04 福建诺德生物科技有限责任公司 Agricultural combination solvent and application thereof
CN103224615A (en) * 2013-04-28 2013-07-31 长兴化学工业(广东)有限公司 Alkyd resin composition and preparation method thereof

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