CN108300396A - A kind of preparation method of viscous snout moth's larva glue - Google Patents
A kind of preparation method of viscous snout moth's larva glue Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J167/00—Adhesives based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Adhesives based on derivatives of such polymers
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Abstract
The invention discloses a kind of preparation methods of viscous snout moth's larva glue, belong to pest control technical field.The present invention takes 1,13 tridecandioic acids that tetrahydrofuran is added, hexamethylene mixing is added in dried object, takes pyridine chlorochromate that rotary evaporation object, dichloromethane is added, it is stirred, it filters, is washed with anhydrous ether, rotary evaporation, it is dry, dried base object is obtained, takes methyltriphenylphospbromide bromide phosphorus that tetrahydrofuran is added, is passed through nitrogen, potassium tert-butoxide mixing is added, mixed matrix object is obtained；It takes waterless cobaltous chloride by tetrahydrofuran mixing is added, takes soybean oil that glycerine is added, be passed through nitrogen, be warming up to, add castor oil, big calcium oxide, phthalic anhydride and dimethylbenzene, be cooled to room temperature, obtain cooling thing；Wheat drying is taken, is pulverized and sieved, sieving particle is collected, takes sieving particle that dichloromethane mixing is added, filtering takes filtrate decompression to distill, and concentrates, obtains concentrated extract, takes cooling thing, concentration to glue snout moth's larva matrix body object, concentrated extract mixing, obtains viscous snout moth's larva glue.
Description
Technical field
The invention belongs to pest control technical fields, and in particular to a kind of preparation method of viscous snout moth's larva glue.
Background technology
Snout moth's larva is the pest of rice, belongs to Lepidoptera.Snout moth's larva is exactly the general designation of phosphorus wing order Glossata Pyralidae insect.China
Frequent species have：The yellow rice borer of Pyralidae, brown side snout moth's larva, striped rice borer, goldrimmed moth and Noctuidae pink rice borer.Yellow rice borer, two change
Snout moth's larva and pink rice borer are the historic major pests of rice.Life habit with the snout moth's larva of rice is similar a bit, if snout moth is all daytime
It lies concealed between standing grain clump or between thick grass, night goes out activity；And there is phototaxis and tend to the habit laid eggs in light green rice strain；In Rice Growing
In the case that phase is inconsistent, snout moth's larva is then more with the oviposition in tiller and incubation period；The larva just come out by egg hatching, cries ant
Snout moth's larva all bores the food rice heart；After larva is aging, hides more and pupate in rice strain lower part.
Current plant insect is to the harm of China's agriculture and forestry except directly caused by feeding in addition to production loss, additionally it is possible to propagate and plant
Object disease causes serious economic loss to agriculture and forestry production.Forest and fruit tree pest insect harm be influence production and fruit farming an important factor for it
One, China is every year since pest damage causes economic loss to be up to tens billion of members.In recent years due to largely having used all kinds of agricultures
Medicine not only makes target pest produce extremely strong drug resistance, becomes refractory pests so that the effect of tree crown spraying prevention is beaten greatly
Discount endangers the normal growth of agriculture and forestry throughout the year, while often causing serious air, soil and water pollution, also at agricultural production
The high reason of persticide residue in product has seriously affected sound development and the agricultural product inlet and outlet trade of China's agriculture and forestry
Easily.With the development of society, enhancing of the people to environmental consciousness, people gradually have found can be to environment and ecology using chemical pesticide
System generates destructive influences.So-called non-environmental pollution control method refers to control measure to people, animal, fowl, fish, honeybee and beneficial
Insect（That is the natural enemy of pest）Safe fanout free region, while to the ecological balance without destruction, agricultural product, which meet pollution-less agriculture, to be wanted
It asks.So the prevention now for the pest for influencing agriculture and forestry production is also non-harmful anti-by relying on chemical method to turn to merely
Control method.
For the insect sticker of pest control, there are two main classes on the market at present：First, being applied directly to the pest activities such as trunk
Pest is clung in position by its viscosity, makes its death, reaches the purpose for controlling its harm, and another kind is with attractant or color etc.
In conjunction with attracting pests are clung.Above-mentioned insect sticker has a certain effect, but using more insect sticker be it is solvent type,
Its smell choke people and existing insect sticker some it is not anti-oxidant, be dried quickly, lose viscosity.Therefore, it is necessary to a kind of at low cost, sticky
Strong and lasting insect sticker product.
Invention content
The technical problems to be solved by the invention：It is solvent type, smell for more viscous dark shellac is used at present
People, the adhesive tension of choking are poor, are dried quickly, lose the problem of viscosity, provide a kind of preparation method of viscous snout moth's larva glue.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of viscous snout moth's larva glue, which is characterized in that the preparation method includes the following steps：
（1）Take 1,13- tridecandioic acids in mass ratio 1：5 are added tetrahydrofuran, are passed through nitrogen, are stirred, add 1,13-
The lithium aluminium hydride reduction of tridecandioic acid quality 50 ~ 60%, be warming up to 25 ~ 30 DEG C holding 10 ~ 12h, obtain mixture A, take mixture A by
Mass ratio 5：2 are added the mixed in hydrochloric acid that mass fraction is 10%, filter, filter residue A is taken to be washed with ethyl acetate, and rotary evaporation is done
It is dry, obtain dried object；
（2）Take dried object in mass ratio 1：35 ~ 40 are added hexamethylene mixing, obtain mixed liquor, according to the mass fraction, take 40 ~ 50 parts
The sulfuric acid mixing of mixed liquor, 15 ~ 20 parts of glacial acetic acid, 20 ~ 30 parts of water, 0.08 ~ 0.1 part of mass fraction 80%, reacts, stands, remove
Miscellaneous, rotary evaporation obtains rotary evaporation object；
（3）Take pyridine chlorochromate in mass ratio 3：3：50 are added rotary evaporation object, dichloromethane, are stirred, and filter, take filter residue
B is washed with anhydrous ether, rotary evaporation, dry, is obtained dried base object, is taken methyltriphenylphospbromide bromide phosphorus in mass ratio 2：20~25
Tetrahydrofuran is added, is passed through nitrogen, adds the potassium tert-butoxide mixing of methyltriphenylphospbromide bromide phosphorus quality 25 ~ 30%, obtains mixed base
Body object；
（4）Take dried base object in mass ratio 3：50 are added tetrahydrofuran, are stirred 15 ~ 20min in -25 ~ 20 DEG C, add
The mixed matrix object of 20 ~ 30 times of dried base amount of substance, reaction, obtains reactant, takes reactant in mass ratio 1：4 are added quality point
Number is 37% ammonium chloride solution, obtains reaction mixture, extracts reaction mixture with anhydrous ether, takes extract liquor rotary evaporation, dense
Contracting, obtains concentrate；
（5）Take waterless cobaltous chloride in mass ratio 1：50 be added tetrahydrofurans mixing, be passed through nitrogen, add water cobalt chloride quality 4 ~
5 times of triphenylphosphine keeps 20 ~ 30min, obtains mixture B, according to the mass fraction, take 30 ~ 40 parts of mixture B, 0.04 ~ 0.05
Part sodium borohydride, 0.4 ~ 0.6 part of concentrate, 5 ~ 7 parts of tetrahydrofurans, are stirred to react 5 ~ 7h in -10 ~ -5 DEG C, obtain reaction stirred,
Take reaction stirred in mass ratio 1：10 are added ether extraction, and rotary evaporation is concentrated under reduced pressure, and must concentrate viscous snout moth's larva matrix body object,
It is spare；
（6）Take soybean oil in mass ratio 3：1 is added glycerine, is passed through nitrogen, is warming up to 160 ~ 170 DEG C of 1 ~ 2h of holding, adds
The castor oil of soybean oil quality 50 ~ 60%, the calcium oxide of soybean oil quality 0.1 ~ 0.3% keep the temperature 3 ~ 4h in 210 ~ 220 DEG C, cooling,
The dimethylbenzene of the phthalic anhydride and castor-oil plant oil quality 60 ~ 80% of 1.5 ~ 2 times of castor-oil plant oil quality is added, in 210 ~ 220 DEG C of stirrings
Mixing, is cooled to room temperature, obtains cooling thing；
（7）It takes wheat drying, crushing to sieve with 100 mesh sieve, collects sieving particle, take sieving particle in mass ratio 1：10 are added dichloromethane
Alkane mixes, and holding 18 ~ for 24 hours, filtering takes filtrate decompression to distill, and concentrates, obtains concentrated extract, according to the mass fraction, take 10 ~ 15
Part cooling thing, 6 ~ 8 parts of steps（5）Snout moth's larva matrix body object, 3 ~ 5 parts of concentrated extract mixing are glued in spare concentration, are kept 1 ~ 2h, are obtained
Viscous snout moth's larva glue.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention selects 1,13- tridecandioic acids cheap and easy to get as raw material for snout moth's larva evil, by carboxyl reduction, unilateral
The processes such as esterification, PCC oxidations, Witting reactions, isomerization are reacted, a kind of parapheromone for inducing snout moth's larva of synthesis,
It lures male worm with the advantages such as of low cost, yield is higher, mild condition, concentration, utilizes the work in viscous snout moth's larva glue
Property ingredient clings male worm, causes female male worm Mating opportunity to largely reduce, reduces the ability to raise up seed, such pest population is close
Degree drastically declines, to achieve the purpose that control pest；
（2）The present invention carries out reaction modifying by the soybean oil of semi-drying and the castor oil bi-component of non-drying to alkyd resin,
Alkyd resin molecular backbone is polar aromatic ring polyester, and side chain is nonpolar aliphatic acid, is adjusted by the oil content of aliphatic acid poly-
Ester ratio makes double bond contained by resin increase using soybean oil, the castor oil compared with long oil, and non-drying is preferable, but simultaneously because
Relative response functional group is reduced in molecular resin, and the surface tack time is long, extends the viscous force time, will not be dried, lose viscosity,
Extension that will not be at any time causes mythimna separata effect to decline, and on the one hand it will not lure ingredient to chemically react with snout moth's larva, also not
It can promote to bring it about isomerization, can will effectively lure ingredient to be wrapped in inside viscous snout moth's larva glue, on the other hand, to environment without dirt
Dye, not will produce penetrating odor；
（3）The present invention also adds broken wheat extract, the auxiliary inducing substance of the parapheromone as snout moth's larva, volatile flavor object
Matter can act synergistically with pheromones, enhance the attracting action to snout moth's larva, the neuron of the trichoid sensillum of male worm is to certain plants
Object odoring substance has reaction, the neuron of pheromone receptor that can react plant scent the receptor for showing plant scent at this
On a little neurons, specific plant scent can selectively stimulus information element receptor neuron, and then influence insect to property
The tentaculum electric potential and behavior reaction of pheromones, increase mythimna separata efficiency, are more advantageous to prevention snout moth's larva evil.
Specific implementation mode
A kind of preparation method of viscous snout moth's larva glue, includes the following steps：
（1）Take 1,13- tridecandioic acids in mass ratio 1：5 are added tetrahydrofurans, are passed through nitrogen, it is stirred 20 in -1 ~ 0 DEG C ~
30min adds the lithium aluminium hydride reduction of 1,13- tridecandioic acids quality 50 ~ 60%, is warming up to 25 ~ 30 DEG C of 10 ~ 12h of holding, obtains mixed
Object A is closed, mixture A in mass ratio 5 is taken：2 are added the mixed in hydrochloric acid that mass fraction is 10%, filter, take filter residue A ethyl acetate
Washing, rotary evaporation is dry, obtains dried object；
（2）Take dried object in mass ratio 1：35 ~ 40 are added hexamethylene mixing, keep 15 ~ 20min, mixed liquor are obtained, by mass fraction
Meter takes the sulfuric acid of 40 ~ 50 portions of mixed liquors, 15 ~ 20 parts of glacial acetic acid, 20 ~ 30 parts of water, 0.08 ~ 0.1 part of mass fraction 80% to mix, in
50 ~ 55 DEG C reaction 8 ~ 10h, stand, take supernatant successively through mass fraction be 6 ~ 8% sodium bicarbonate solution, mass fraction be
26% sodium chloride solution removal of impurities, rotary evaporation obtain rotary evaporation object；
（3）Take pyridine chlorochromate in mass ratio 3：3：50 are added rotary evaporation objects, dichloromethane, it is stirred 4 in 25 ~ 35 DEG C ~
5h, filters, filter residue B is taken to be washed with anhydrous ether, and rotary evaporation is dry, obtains dried base object, take methyltriphenylphospbromide bromide phosphorus by
Mass ratio 2：20 ~ 25 are added tetrahydrofuran, are passed through nitrogen, add the potassium tert-butoxide of methyltriphenylphospbromide bromide phosphorus quality 25 ~ 30%
20 ~ 30min is mixed, mixed matrix object is obtained；
（4）Take dried base object in mass ratio 3：50 are added tetrahydrofuran, are stirred 15 ~ 20min in -25 ~ 20 DEG C, add
The mixed matrix object of 20 ~ 30 times of dried base amount of substance reacts 4 ~ 6h, obtains reactant, take reactant in mass ratio 1：4 are added matter
The ammonium chloride solution that score is 37% is measured, reaction mixture is obtained, reaction mixture is extracted with anhydrous ether, extract liquor rotation is taken to steam
Hair, concentration, obtains concentrate；
（5）Take waterless cobaltous chloride in mass ratio 1：50 be added tetrahydrofurans mixing, be passed through nitrogen, add water cobalt chloride quality 4 ~
5 times of triphenylphosphine keeps 20 ~ 30min, obtains mixture B, according to the mass fraction, take 30 ~ 40 parts of mixture B, 0.04 ~ 0.05
Part sodium borohydride, 0.4 ~ 0.6 part of concentrate, 5 ~ 7 parts of tetrahydrofurans, are stirred to react 5 ~ 7h in -10 ~ -5 DEG C, obtain reaction stirred,
Take reaction stirred in mass ratio 1：10 are added ether extraction, and rotary evaporation is concentrated under reduced pressure, and must concentrate viscous snout moth's larva matrix body object,
It is spare；
（6）Take soybean oil in mass ratio 3：1 is added glycerine, is passed through nitrogen, is warming up to 160 ~ 170 DEG C of 1 ~ 2h of holding, adds
The calcium oxide of the castor oil and soybean oil quality 0.1 ~ 0.3% of soybean oil quality 50 ~ 60% keeps the temperature 3 ~ 4h in 210 ~ 220 DEG C, cooling
To 150 ~ 160 DEG C, the dimethylbenzene of the phthalic anhydride and castor-oil plant oil quality 60 ~ 80% of 1.5 ~ 2 times of castor-oil plant oil quality is added, in
210 ~ 220 DEG C are stirred 3 ~ 5h, are cooled to room temperature, obtain cooling thing；
（7）It takes wheat drying, crushing to sieve with 100 mesh sieve, collects sieving particle, take sieving particle in mass ratio 1：10 are added dichloromethane
Alkane mixes, and holding 18 ~ for 24 hours, filtering takes filtrate decompression to distill, and concentrates, obtains concentrated extract, according to the mass fraction, take 10 ~ 15
Part cooling thing, 6 ~ 8 parts of steps（5）Snout moth's larva matrix body object, 3 ~ 5 parts of concentrated extract mixing are glued in spare concentration, are kept 1 ~ 2h, are obtained
Viscous snout moth's larva glue.
A kind of preparation method of viscous snout moth's larva glue, includes the following steps：
（1）Take 1,13- tridecandioic acids in mass ratio 1：5 are added tetrahydrofuran, are passed through nitrogen, 20min is stirred in -1 DEG C,
The lithium aluminium hydride reduction for adding 1,13- tridecandioic acids quality 50% is warming up to 25 DEG C of holding 10h, obtains mixture A, take mixture A
In mass ratio 5：2 are added the mixed in hydrochloric acid that mass fraction is 10%, filter, filter residue A is taken to be washed with ethyl acetate, and rotary evaporation is done
It is dry, obtain dried object；
（2）Take dried object in mass ratio 1：35 are added hexamethylene mixing, keep 15min, obtain mixed liquor, according to the mass fraction, take
The sulfuric acid mixing of 40 portions of mixed liquors, 15 parts of glacial acetic acid, 20 parts of water, 0.08 part of mass fraction 80% stands, takes in 50 DEG C of reaction 8h
The sodium chloride solution removal of impurities that sodium bicarbonate solution that supernatant is successively 6% through mass fraction, mass fraction are 26%, rotation are steamed
Hair, obtains rotary evaporation object；
（3）Take pyridine chlorochromate in mass ratio 3：3：50 are added rotary evaporation object, dichloromethane, and 4h is stirred in 25 DEG C, take out
Filter, takes filter residue B to be washed with anhydrous ether, rotary evaporation, dry, obtains dried base object, takes methyltriphenylphospbromide bromide phosphorus by quality
Than 2：20 are added tetrahydrofuran, are passed through nitrogen, add the potassium tert-butoxide mixing 20min of methyltriphenylphospbromide bromide phosphorus quality 25%,
Obtain mixed matrix object；
（4）Take dried base object in mass ratio 3：50 are added tetrahydrofuran, are stirred 15min in -25 DEG C, add dry base
The mixed matrix object of 20 times of body amount of substance reacts 4h, obtains reactant, take reactant in mass ratio 1：4 addition mass fractions are 37%
Ammonium chloride solution, obtain reaction mixture, with anhydrous ether extract reaction mixture, take extract liquor rotary evaporation, concentrate, obtain dense
Contracting object；
（5）Take waterless cobaltous chloride in mass ratio 1：50 are added tetrahydrofuran mixing, are passed through nitrogen, add water cobalt chloride quality 4
Times triphenylphosphine, keep 20min, obtain mixture B, according to the mass fraction, take 30 parts of mixture B, 0.04 part of sodium borohydride,
0.4 part of concentrate, 5 parts of tetrahydrofurans, are stirred to react 5h in -10 DEG C, obtain reaction stirred, take reaction stirred in mass ratio 1：
10 are added ether extraction, and rotary evaporation is concentrated under reduced pressure, and must concentrate viscous snout moth's larva matrix body object, spare；
（6）Take soybean oil in mass ratio 3：1 is added glycerine, is passed through nitrogen, is warming up to 160 DEG C of holding 1h, adds soybean oil
The calcium oxide of the castor oil and soybean oil quality 0.1% of quality 50% keeps the temperature 3h in 210 DEG C, is cooled to 150 DEG C, castor oil is added
The dimethylbenzene of the phthalic anhydride and castor-oil plant oil quality 60% that 1.5 times of quality is stirred 3h in 210 DEG C, is cooled to room temperature,
Obtain cooling thing；
（7）It takes wheat drying, crushing to sieve with 100 mesh sieve, collects sieving particle, take sieving particle in mass ratio 1：10 are added dichloromethane
Alkane mixes, and keeps 18h, filtering that filtrate decompression is taken to distill, concentrates, obtain concentrated extract, according to the mass fraction, take 10 parts of coolings
Object, 6 parts of steps（5）Snout moth's larva matrix body object, 3 parts of concentrated extract mixing are glued in spare concentration, are kept 1h, are obtained viscous snout moth's larva glue.
A kind of preparation method of viscous snout moth's larva glue, includes the following steps：
（1）Take 1,13- tridecandioic acids in mass ratio 1：5 are added tetrahydrofuran, are passed through nitrogen, 30min is stirred in 0 DEG C,
The lithium aluminium hydride reduction for adding 1,13- tridecandioic acids quality 60% is warming up to 30 DEG C of holding 12h, obtains mixture A, take mixture A
In mass ratio 5：2 are added the mixed in hydrochloric acid that mass fraction is 10%, filter, filter residue A is taken to be washed with ethyl acetate, and rotary evaporation is done
It is dry, obtain dried object；
（2）Take dried object in mass ratio 1：40 are added hexamethylene mixing, keep 20min, obtain mixed liquor, according to the mass fraction, take
The sulfuric acid mixing of 50 portions of mixed liquors, 20 parts of glacial acetic acid, 30 parts of water, 0.1 part of mass fraction 80% stands, takes in 55 DEG C of reaction 10h
The sodium chloride solution removal of impurities that sodium bicarbonate solution that supernatant is successively 8% through mass fraction, mass fraction are 26%, rotation are steamed
Hair, obtains rotary evaporation object；
（3）Take pyridine chlorochromate in mass ratio 3：3：50 are added rotary evaporation object, dichloromethane, and 5h is stirred in 35 DEG C, take out
Filter, takes filter residue B to be washed with anhydrous ether, rotary evaporation, dry, obtains dried base object, takes methyltriphenylphospbromide bromide phosphorus by quality
Than 2：25 are added tetrahydrofuran, are passed through nitrogen, add the potassium tert-butoxide mixing 30min of methyltriphenylphospbromide bromide phosphorus quality 30%,
Obtain mixed matrix object；
（4）Take dried base object in mass ratio 3：50 are added tetrahydrofuran, are stirred 20min in 20 DEG C, add dry base
The mixed matrix object of 30 times of body amount of substance reacts 6h, obtains reactant, take reactant in mass ratio 1：4 addition mass fractions are 37%
Ammonium chloride solution, obtain reaction mixture, with anhydrous ether extract reaction mixture, take extract liquor rotary evaporation, concentrate, obtain dense
Contracting object；
（5）Take waterless cobaltous chloride in mass ratio 1：50 are added tetrahydrofuran mixing, are passed through nitrogen, add water cobalt chloride quality 5
Times triphenylphosphine, keep 30min, obtain mixture B, according to the mass fraction, take 40 parts of mixture B, 0.05 part of sodium borohydride,
0.6 part of concentrate, 7 parts of tetrahydrofurans, are stirred to react 7h in -5 DEG C, obtain reaction stirred, take reaction stirred in mass ratio 1：
10 are added ether extraction, and rotary evaporation is concentrated under reduced pressure, and must concentrate viscous snout moth's larva matrix body object, spare；
（6）Take soybean oil in mass ratio 3：1 is added glycerine, is passed through nitrogen, is warming up to 170 DEG C of holding 2h, adds soybean oil
The calcium oxide of the castor oil and soybean oil quality 0.3% of quality 60% keeps the temperature 4h in 220 DEG C, is cooled to 160 DEG C, castor oil is added
The dimethylbenzene of the phthalic anhydride and castor-oil plant oil quality 80% that 2 times of quality is stirred 5h in 220 DEG C, is cooled to room temperature, obtains
Cooling thing；
（7）It takes wheat drying, crushing to sieve with 100 mesh sieve, collects sieving particle, take sieving particle in mass ratio 1：10 are added dichloromethane
Alkane mixes, and keeps for 24 hours, and filtering takes filtrate decompression to distill, and concentrates, obtains concentrated extract, according to the mass fraction, take 15 parts of coolings
Object, 8 parts of steps（5）Snout moth's larva matrix body object, 5 parts of concentrated extract mixing are glued in spare concentration, are kept 2h, are obtained viscous snout moth's larva glue.
A kind of preparation method of viscous snout moth's larva glue, includes the following steps：
（1）Take 1,13- tridecandioic acids in mass ratio 1：5 are added tetrahydrofuran, are passed through nitrogen, 25min is stirred in 0 DEG C,
The lithium aluminium hydride reduction for adding 1,13- tridecandioic acids quality 55% is warming up to 27 DEG C of holding 11h, obtains mixture A, take mixture A
In mass ratio 5：2 are added the mixed in hydrochloric acid that mass fraction is 10%, filter, filter residue A is taken to be washed with ethyl acetate, and rotary evaporation is done
It is dry, obtain dried object；
（2）Take dried object in mass ratio 1：37 are added hexamethylene mixing, keep 17.5min, obtain mixed liquor, according to the mass fraction,
It takes the sulfuric acid of 45 portions of mixed liquors, 17.5 parts of glacial acetic acid, 25 parts of water, 0.09 part of mass fraction 80% to mix, 9h is reacted in 53 DEG C, it is quiet
It sets, takes the sodium chloride solution that sodium bicarbonate solution, mass fraction that supernatant is successively 7% through mass fraction are 26% to clean, rotation
Turn evaporation, obtains rotary evaporation object；
（3）Take pyridine chlorochromate in mass ratio 3：3：50 are added rotary evaporation object, dichloromethane, and 4.5h is stirred in 30 DEG C,
It filters, filter residue B is taken to be washed with anhydrous ether, rotary evaporation is dry, obtains dried base object, takes methyltriphenylphospbromide bromide phosphorus by matter
Measure ratio 2：22.5 are added tetrahydrofuran, are passed through nitrogen, add the potassium tert-butoxide mixing of methyltriphenylphospbromide bromide phosphorus quality 27.5%
25min obtains mixed matrix object；
（4）Take dried base object in mass ratio 3：50 are added tetrahydrofuran, are stirred 17.5min in 5 DEG C, add dry base
The mixed matrix object of 25 times of body amount of substance reacts 5h, obtains reactant, take reactant in mass ratio 1：4 addition mass fractions are 37%
Ammonium chloride solution, obtain reaction mixture, with anhydrous ether extract reaction mixture, take extract liquor rotary evaporation, concentrate, obtain dense
Contracting object；
（5）Take waterless cobaltous chloride in mass ratio 1：50 are added tetrahydrofuran mixing, are passed through nitrogen, add water cobalt chloride quality
4.5 times of triphenylphosphine keeps 25min, obtains mixture B, according to the mass fraction, take 35 parts of mixture B, 0.045 part of hydroboration
Sodium, 0.5 part of concentrate, 6 parts of tetrahydrofurans, are stirred to react 6h in -7 DEG C, obtain reaction stirred, take reaction stirred in mass ratio
1：10 are added ether extraction, and rotary evaporation is concentrated under reduced pressure, and must concentrate viscous snout moth's larva matrix body object, spare；
（6）Take soybean oil in mass ratio 3：1 is added glycerine, is passed through nitrogen, is warming up to 165 DEG C of holding 1.5h, adds soybean
The calcium oxide of the castor oil and soybean oil quality 0.2% of oil quality 55% keeps the temperature 3.5h in 215 DEG C, is cooled to 155 DEG C, castor is added
The dimethylbenzene of the phthalic anhydride and castor-oil plant oil quality 70% that 1.7 times of sesame oil quality is stirred 4h in 215 DEG C, is cooled to room
Temperature obtains cooling thing；
（7）It takes wheat drying, crushing to sieve with 100 mesh sieve, collects sieving particle, take sieving particle in mass ratio 1：10 are added dichloromethane
Alkane mixes, and keeps 21h, filtering that filtrate decompression is taken to distill, concentrates, obtain concentrated extract, according to the mass fraction, take 2.5 parts of coolings
Object, 7 parts of steps（5）Snout moth's larva matrix body object, 4 parts of concentrated extract mixing are glued in spare concentration, are kept 1.5h, are obtained viscous snout moth's larva glue.
Comparative example：The insect sticker of company of Shenzhen production.
20cm × 30cm plank is selected first, and the thin fixed plank of rod support of bamboo and wood is used in combination, respectively prepares the present invention
Viscous snout moth's larva glue and the insect sticker of comparative example be evenly applied to plank two sides, control coating thickness is 0.8mm, will finally be fixed
Plank be inserted into field, be uniformly inserted into 20 pieces of planks per acre, after being inserted into, detect to the control effect of snout moth's larva, detection knot
Fruit is shown in Table 1.
Table 1：
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Snout moth's larva eradicative rate % | 98.9 | 98.7 | 98 | 74~76 |
| Flies eradicative rate % | 94 | 95 | 94 | 80~82 |
| Persistence（Month） | 15 | 14.5 | 15.1 | 4~6 |
| Smell | It is thin | It is thin | It is thin | It is pungent |
In summary, viscous snout moth's larva glue of the invention is apparent to the function and effect of snout moth's larva, comprehensive performance also superior to presently commercially available product,
Be worth promoting use.
Claims (1)
1. a kind of preparation method of viscous snout moth's larva glue, which is characterized in that the preparation method includes the following steps：
（1）Take 1,13- tridecandioic acids in mass ratio 1：5 are added tetrahydrofuran, are passed through nitrogen, are stirred, add 1,13-
The lithium aluminium hydride reduction of tridecandioic acid quality 50 ~ 60%, be warming up to 25 ~ 30 DEG C holding 10 ~ 12h, obtain mixture A, take mixture A by
Mass ratio 5：2 are added the mixed in hydrochloric acid that mass fraction is 10%, filter, filter residue A is taken to be washed with ethyl acetate, and rotary evaporation is done
It is dry, obtain dried object；
（2）Take dried object in mass ratio 1：35 ~ 40 are added hexamethylene mixing, obtain mixed liquor, according to the mass fraction, take 40 ~ 50 parts
The sulfuric acid mixing of mixed liquor, 15 ~ 20 parts of glacial acetic acid, 20 ~ 30 parts of water, 0.08 ~ 0.1 part of mass fraction 80%, reacts, stands, remove
Miscellaneous, rotary evaporation obtains rotary evaporation object；
（3）Take pyridine chlorochromate in mass ratio 3：3：50 are added rotary evaporation object, dichloromethane, are stirred, and filter, take filter residue
B is washed with anhydrous ether, rotary evaporation, dry, is obtained dried base object, is taken methyltriphenylphospbromide bromide phosphorus in mass ratio 2：20~25
Tetrahydrofuran is added, is passed through nitrogen, adds the potassium tert-butoxide mixing of methyltriphenylphospbromide bromide phosphorus quality 25 ~ 30%, obtains mixed base
Body object；
（4）Take dried base object in mass ratio 3：50 are added tetrahydrofuran, are stirred 15 ~ 20min in -25 ~ 20 DEG C, add
The mixed matrix object of 20 ~ 30 times of dried base amount of substance, reaction, obtains reactant, takes reactant in mass ratio 1：4 are added quality point
Number is 37% ammonium chloride solution, obtains reaction mixture, extracts reaction mixture with anhydrous ether, takes extract liquor rotary evaporation, dense
Contracting, obtains concentrate；
（5）Take waterless cobaltous chloride in mass ratio 1：50 be added tetrahydrofurans mixing, be passed through nitrogen, add water cobalt chloride quality 4 ~
5 times of triphenylphosphine keeps 20 ~ 30min, obtains mixture B, according to the mass fraction, take 30 ~ 40 parts of mixture B, 0.04 ~ 0.05
Part sodium borohydride, 0.4 ~ 0.6 part of concentrate, 5 ~ 7 parts of tetrahydrofurans, are stirred to react 5 ~ 7h in -10 ~ -5 DEG C, obtain reaction stirred,
Take reaction stirred in mass ratio 1：10 are added ether extraction, and rotary evaporation is concentrated under reduced pressure, and must concentrate viscous snout moth's larva matrix body object,
It is spare；
（6）Take soybean oil in mass ratio 3：1 is added glycerine, is passed through nitrogen, is warming up to 160 ~ 170 DEG C of 1 ~ 2h of holding, adds
The castor oil of soybean oil quality 50 ~ 60%, the calcium oxide of soybean oil quality 0.1 ~ 0.3% keep the temperature 3 ~ 4h in 210 ~ 220 DEG C, cooling,
The dimethylbenzene of the phthalic anhydride and castor-oil plant oil quality 60 ~ 80% of 1.5 ~ 2 times of castor-oil plant oil quality is added, in 210 ~ 220 DEG C of stirrings
Mixing, is cooled to room temperature, obtains cooling thing；
（7）It takes wheat drying, crushing to sieve with 100 mesh sieve, collects sieving particle, take sieving particle in mass ratio 1：10 are added dichloromethane
Alkane mixes, and holding 18 ~ for 24 hours, filtering takes filtrate decompression to distill, and concentrates, obtains concentrated extract, according to the mass fraction, take 10 ~ 15
Part cooling thing, 6 ~ 8 parts of steps（5）Snout moth's larva matrix body object, 3 ~ 5 parts of concentrated extract mixing are glued in spare concentration, are kept 1 ~ 2h, are obtained
Viscous snout moth's larva glue.
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| US4122073A (en) * | 1977-08-01 | 1978-10-24 | National Starch And Chemical Corporation | Thermoplastic copolyesters prepared from aromatic dicarboxylic acid, substituted succinic acid or anhydride, a glycol and a polymeric polyol and the use thereof in adhesives |
| CN102181255A (en) * | 2011-04-12 | 2011-09-14 | 沈阳化工大学 | Method for preparing hot-melt pressure sensitive adhesives by using illegal cooking oil |
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