CN107033184A - The preparation method and its product of a kind of dibutyl tin laurate - Google Patents
The preparation method and its product of a kind of dibutyl tin laurate Download PDFInfo
- Publication number
- CN107033184A CN107033184A CN201710366937.4A CN201710366937A CN107033184A CN 107033184 A CN107033184 A CN 107033184A CN 201710366937 A CN201710366937 A CN 201710366937A CN 107033184 A CN107033184 A CN 107033184A
- Authority
- CN
- China
- Prior art keywords
- dibutyl tin
- tin laurate
- laurate
- catalyst
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/22—Tin compounds
- C07F7/2208—Compounds having tin linked only to carbon, hydrogen and/or halogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention belongs to synthesize field, it is related to the preparation method and its product of a kind of dibutyl tin laurate.The preparation method of the dibutyl tin laurate, at least comprises the following steps：Laurate, dibutyl tin dichloride, ethanol are sequentially added into reactor, wherein, the mol ratio 2 between laurate, dichloro dibutyl tin, ethanol：1：10, after stirring, sequentially add catalyst, trimethylolpropane tris (mercaptopropionic acid ester), at 40 DEG C, 30~60min of stirring reaction, then sodium hydroxide solution is added, the pH value of regulation reaction is 7, and then at 40 DEG C, 1~3h of stirring reaction, after reaction terminates, reaction solution is obtained；Then the solvent in reaction solution is distilled out, obtains product, after product is washed, be drying to obtain dibutyl tin laurate；The catalyst is that N (2 aminoethyl) 3 aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
Description
Technical field
The invention belongs to synthesize field, it is related to the preparation method and its product of a kind of dibutyl tin laurate.
Background technology
Polyvinyl chloride (PVC) is one of big general-purpose plastics in the world five, and greatly, application is extremely wide for yield consumption.Polychlorostyrene second
Alkene (PVC) plastics have the advantages that self-extinguishment, higher fire-retardant, wear-resisting, intensity, electrical insulating property and chemical stability are preferable, and price
Cheap, using quite varied, but its heat endurance is poor, and heat stabilizer must be added in process, with prevent PVC discolorations,
Degraded.Correspondingly, the development of PVC heat stabilizer and the development of polrvinyl chloride product are closely bound up.
Organo-tin het stabilizer is one of higher and very promising PVC heat stabilizer of thermally-stabilised efficiency, it efficiently,
Low (nothing) poison, be particularly suitable for use in transparent and hygienic articles.In China, New Heat Stabilizer production does not catch up with PVC much with application
Industrial expansion.Accelerate, strengthen the development and application research of new organo-tin het stabilizer has turned into a kind of inevitable.
Dibutyl tin laurate is a kind of organotin additive, and the higher boiling multipurpose circulated on the market is organotin catalyzed
Agent dibutyl tin laurate is handled by special liquefaction, is light yellow or colourless oil liquid under normal temperature, low
Temperature is into white crystalline body, available for igelite auxiliary agent, with excellent lubricity, transparent, weatherability.Halophile is dirty
Dye is preferable.The used as stabilizers in soft transparent product, makees highly-efficient lubricant in hard transparent product, also acts as acrylate
The catalyst of rubber and carboxylic rubber cross-linking reaction, polyurethane foam plastics synthesis and polyester synthesis, room temperature vulcanized silicone rubber is urged
Agent.
At present, in the prior art, in the building-up process of dibutyl tin laurate, catalytic efficiency is relatively low, thus non-
Often need by the improvement of synthesis technique to synthesize a new dibutyl tin laurate, make it that there is PVC preferable
Thermal stability.
The content of the invention
In order to solve the above-mentioned technical problem, the first aspect of the invention provides a kind of system of dibutyl tin laurate
Preparation Method, at least comprises the following steps：
Laurate, dibutyl tin dichloride, ethanol are sequentially added into reactor, wherein, laurate, dichloro dibutyl
Mol ratio 2 between tin, ethanol：1：10, after stirring, sequentially add the catalyst, (sulfydryl third of trimethylolpropane-three
Acid esters), at 40 DEG C, then 30~60min of stirring reaction adds sodium hydroxide solution, the pH value of regulation reaction is 7, and
Then at 40 DEG C, 1~3h of stirring reaction after reaction terminates, obtains reaction solution；Then the solvent in reaction solution is distilled out,
Product is obtained, after product is washed, dibutyl tin laurate is drying to obtain；The catalyst be N- (2- aminoethyls)-
3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
As a kind of preferred technical scheme of the present invention, in the catalyst, N- (2- aminoethyls) -3- aminopropyl trimethoxies
Weight ratio between base silane and mesoporous silicon oxide is：(1~3)：10.
As a kind of preferred technical scheme of the present invention, the mesoporous silicon oxide is selected from：MCM-41、MCM-48、MCM-
50th, any one or a few the mixing in SBA-15, SBA-16.
As a kind of preferred technical scheme of the present invention, the catalyst is that dibutyl tin laurate loads N- (2- ammonia
Ethyl) -3- aminopropyl trimethoxysilanes modification mesoporous silicon oxide.
As a kind of preferred technical scheme of the present invention, the dibutyl tin laurate and N- (2- aminoethyls) -3- ammonia
Propyl trimethoxy silicane be modified mesoporous silicon oxide between weight ratio be：1：50.
As a kind of preferred technical scheme of the present invention, the catalyst, trimethylolpropane-three (mercaptopropionic acid ester) it
Between weight ratio be 100：3.
The second aspect of the invention provides the obtained dibutyl tin laurate of the above method in heat stabilizer, catalysis
Agent, drier, the application of dye field.
The third aspect of the invention provides a kind of dibutyl tin laurate composite thermal stabilizer, at least including following
Raw material,
100 parts of dibutyl tin laurate；
1~10 part of epoxidized linseed oil；
5 parts of beta-diketon；
The preparation method of the dibutyl tin laurate is as follows：
Laurate, dibutyl tin dichloride, ethanol are sequentially added into reactor, wherein, laurate, dichloro dibutyl
Mol ratio 2 between tin, ethanol：1：10, after stirring, sequentially add the catalyst, (sulfydryl third of trimethylolpropane-three
Acid esters), at 40 DEG C, then 30~60min of stirring reaction adds sodium hydroxide solution, the pH value of regulation reaction is 7, and
Then at 40 DEG C, 1~3h of stirring reaction after reaction terminates, obtains reaction solution；Then the solvent in reaction solution is distilled out,
Product is obtained, after product is washed, dibutyl tin laurate is drying to obtain；The catalyst be N- (2- aminoethyls)-
3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
The fourth aspect of the invention provides a kind of PVC composition, in parts by weight, at least including following raw material,
100 parts of polyvinyl chloride resin；
1~10 part of superbrnaching end-hydroxy polyester；
1~3 part of dibutyl tin laurate.
The fifth aspect of the invention provides a kind of preparation method of PVC composition, at least comprises the following steps：
The polyvinyl chloride resin, superbrnaching end-hydroxy polyester, dibutyl tin laurate of corresponding parts by weight are added to mixed at high speed
In machine, after uniform mixing, 200 DEG C are then placed in again and is kneaded 5~10 minutes in two-roll mill, you can PVC composition is obtained.
The above-mentioned of the application and other features, aspect and advantage is more readily understood with reference to described further below.
Embodiment
The participation in the election detailed description of the invention below for being preferable to carry out method and including embodiment this public affairs can be more easily understood
Open content.A large amount of terms can be referred in description below and claims, these terms are defined as following meanings.
As used herein term " by ... prepare " it is synonymous with "comprising".Term "comprising" used herein, " comprising ",
" having ", " containing " or its any other deformation, it is intended that cover including for non-exclusionism.For example, the combination comprising listed elements
Thing, step, method, product or device are not necessarily limited to those key elements, but can include not expressly listed other key elements or
Such a composition, step, method, product or the intrinsic key element of device." optionally " or " optionally " refer to describe thereafter
Item or event may or may not occur, and the description includes the situation and the situation that does not occur of event that event occurs.
Equivalent, concentration or other values or parameter are excellent with scope, preferred scope or a series of upper limit preferred values and lower limit
During the Range Representation that choosing value is limited, this, which is appreciated that, specifically discloses by any range limit or preferred value and any scope
All scopes that any pairing of lower limit or preferred value is formed, regardless of whether whether the scope separately discloses.For example, when open
During scope " 1 to 5 ", described scope should be interpreted as including scope " 1 to 4 ", " 1 to 3 ", " 1~2 ", " 1~2 and 4~
5 ", " 1~3 and 5 " etc..When number range is described herein, unless otherwise indicated, otherwise the scope is intended to include its end
Value and all integers and fraction within the range.
In order to solve the above-mentioned technical problem, the first aspect of the invention provides a kind of system of dibutyl tin laurate
Preparation Method, at least comprises the following steps：
Laurate, dibutyl tin dichloride, ethanol are sequentially added into reactor, wherein, laurate, dichloro dibutyl
Mol ratio 2 between tin, ethanol：1：10, after stirring, sequentially add the catalyst, (sulfydryl third of trimethylolpropane-three
Acid esters), at 40 DEG C, then 30~60min of stirring reaction adds sodium hydroxide solution, the pH value of regulation reaction is 7, and
Then at 40 DEG C, 1~3h of stirring reaction after reaction terminates, obtains reaction solution；Then the solvent in reaction solution is distilled out,
Product is obtained, after product is washed, dibutyl tin laurate is drying to obtain；The catalyst be N- (2- aminoethyls)-
3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
Term " N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide " refers to N- (2- ammonia
Ethyl) -3- aminopropyl trimethoxysilanes are grafted to the surface of mesoporous silicon oxide, obtained compound.
In a preferred embodiment, the mesoporous silicon oxide is selected from：MCM-41、MCM-48、MCM-50、SBA-
15th, any one or a few the mixing in SBA-16.
In the application, the mesoporous silicon oxide obtains to be commercially available, is purchased from Nanjing Ji Cang nanosecond science and technology Co., Ltd.
In a preferred embodiment, in the catalyst, N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes
Weight ratio between mesoporous silicon oxide is：(1~3)：10.
In a preferred embodiment, the preparation method of the catalyst, at least comprises the following steps：
In the reactor, solvent 100ml toluene and 10g MCM-41, ultrasonic disperse 10min are added, 1g N- are then added
(2- aminoethyls) -3- aminopropyl trimethoxysilanes, add the triethylamine solution that volumetric concentration is 10%, are flowed back at 100 DEG C
2h is reacted, filtering, ethanol is washed 3 times, be dried to obtain N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes and be modified titanium dioxide
Silicon.
Term " trimethylolpropane-three (mercaptopropionic acid ester) " is purchased from western precious biology, and it act as co-catalysis, with catalyst
Catalytic action is played jointly, material conversion efficiency is improved, and reduces the reaction time.
In a kind of most preferred embodiment, the catalyst is that dibutyl tin laurate loads N- (2- ammonia second
Base) -3- aminopropyl trimethoxysilanes modification mesoporous silicon oxide.
" dibutyl tin laurate load N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified mesoporous two to term
Silica " refers to be modified on the surface of mesoporous silicon oxide in catalyst n-(2- aminoethyls) -3- aminopropyl trimethoxysilanes
The a small amount of dibutyl tin laurate of load.
The inventors discovered that, the catalyst through overload dibutyl tin laurate, in the conjunction of dibutyl tin laurate
During, without isolating catalyst from system, due to the presence of catalyst, it can make it that dibutyl tin laurate heat is steady
Agent is determined in PVC compound systems, plays good thermal stability.
In a preferred embodiment, described dibutyl tin laurate load N- (2- aminoethyls) -3- aminopropyls
The preparation method that trimethoxy silane is modified mesoporous silicon oxide is as follows：
By dibutyl tin laurate dissolving in ethanol, it is made into the dibutyl tin laurate that mass fraction is 5% molten
Liquid, then, then addition N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes modification Jie into dibutyl tin laurate solution
Hole silica, is stirred 2 hours at 25 DEG C, stewing process 4 hours, through filtering, washing, dry after obtain di lauric dibutyl
Tin load N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
In a preferred embodiment, the dibutyl tin laurate and N- (2- aminoethyls) -3- aminopropyls three
Methoxy silane be modified mesoporous silicon oxide between weight ratio be：1：50.
In a preferred embodiment, the weight between the catalyst, trimethylolpropane-three (mercaptopropionic acid ester)
Amount is than being 100：3.
The second aspect of the invention provides the obtained dibutyl tin laurate of the above method in heat stabilizer, catalysis
Agent, drier, the application of dye field.
The third aspect of the invention provides a kind of dibutyl tin laurate composite thermal stabilizer, at least including following
Raw material,
100 parts of dibutyl tin laurate；
1~10 part of epoxidized linseed oil；
5 parts of beta-diketon；
The preparation method of the dibutyl tin laurate is as follows：
Laurate, dibutyl tin dichloride, ethanol are sequentially added into reactor, wherein, laurate, dichloro dibutyl
Mol ratio 2 between tin, ethanol：1：10, after stirring, sequentially add the catalyst, (sulfydryl third of trimethylolpropane-three
Acid esters), at 40 DEG C, then 30~60min of stirring reaction adds sodium hydroxide solution, the pH value of regulation reaction is 7, and
Then at 40 DEG C, 1~3h of stirring reaction after reaction terminates, obtains reaction solution；Then the solvent in reaction solution is distilled out,
Product is obtained, after product is washed, dibutyl tin laurate is drying to obtain；The catalyst be N- (2- aminoethyls)-
3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
In a preferred embodiment, in the catalyst, N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes
Weight ratio between mesoporous silicon oxide is：(1~3)：10.
In a preferred embodiment, the mesoporous silicon oxide is selected from：MCM-41、MCM-48、MCM-50、SBA-
15th, any one or a few the mixing in SBA-16.
In a preferred embodiment, the catalyst be dibutyl tin laurate load N- (2- aminoethyls)-
3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
In a preferred embodiment, the dibutyl tin laurate and N- (2- aminoethyls) -3- aminopropyls three
Methoxy silane be modified mesoporous silicon oxide between weight ratio be：1：50.
In a preferred embodiment, the weight between the catalyst, trimethylolpropane-three (mercaptopropionic acid ester)
Amount is than being 100：3.
In a preferred embodiment, the preparation method of the dibutyl tin laurate composite thermal stabilizer is such as
Under：
After the dibutyl tin laurate, epoxidized linseed oil, beta-diketon of corresponding parts by weight uniformly mixing, at 80 DEG C
1h is stirred, room temperature is then cooled to, obtains dibutyl tin laurate composite thermal stabilizer.
The fourth aspect of the invention provides a kind of PVC composition, in parts by weight, at least including following raw material,
100 parts of polyvinyl chloride resin；
1~10 part of superbrnaching end-hydroxy polyester；
1~3 part of dibutyl tin laurate composite thermal stabilizer.
In a preferred embodiment, in the environment-friendly type PVC composition, in addition to auxiliary agent.
What the auxiliary agent can be enumerated has：Antioxidant, plasticizer, fire retardant, filler, ultra-violet absorber, antiseptic, face
Expect, enter delustering agent, weather resisting agent, antistatic agent, anti-coloring agent etc..
What the antioxidant can be enumerated has：Phenolic antioxidant, phosphite ester kind antioxidant, containing in sulphur ester antioxidant
It is at least one.
Phenolic antioxidant can be enumerated：1- hydroxy-3-methyl -4- cumenes, 2,6- DI-tert-butylphenol compounds, the uncles of 2,6- bis-
Butyl -4- ethyl -phenols, BHT, 2,6- di-t-butyl -4- normal-butyls phenol, 4- methylols -2,6- bis-
Tert-butyl phenol, butylhydroxy anisole, 2- (1- methylcyclohexyls) -4,6- xylenols, the tertiary fourths of 2,4- dimethyl -6-
Base phenol, 2- methyl -4,6- dinonyl phenol, 2,6- di-t-butyls-alpha, alpha-dimethyl amino-p-cresol, 2,4,6- tri-butyl benzenes
Double (the octylsulfo) -1,3,5-triazines of phenol, 6- (4- hydroxyl -3,5- di-tert-butyls amido) -2,4-, 4,6- it is double (4- hydroxyl -3,
5- di-t-butyls phenoxy group) -2- n-octylthios -1,3,5-triazines, β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid first
Ester, β-positive octadecanol ester of (4-hydroxyl-3,5-di-tert-butyl-phenyl) propionic acid, styrenated phenol, 4,4 '-dihydroxy connection
Benzene, butylated octylated phenol, butylated stytrene cresols, 2,2 '-methylene bis (4- methyl-6-tert-butylphenols) or 2,
2 '-methylene bis (the 6- tert-butyl group -4- cresols), 2,2 '-methylene bis (4- ethyl -6- tert-butyl phenols), 2,2 '-methylene bis (4- first
Base -6- cyclohexylphenols), 4,4 '-methylene bis (2,6- DI-tert-butylphenol compounds), 2, (6- α-methylbenzyls are to first for 2 '-methylene bis
Phenol), 1,1- double (4- hydroxy benzenes) hexamethylene, 2,2 '-methylene bis (4- methyl -6- (Alpha-Methyl cyclohexyl) phenol) or 2,2 '-two
Hydroxyl -3,3 '-two (Alpha-Methyl cyclohexyl) -5,5 '-dimethyl diphenylmethane, 1,3,5- trimethyls -2,4,6- tri- (3,5- bis-
Tertiary butyl-4-hydroxy benzyl) benzene, 1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyls) butane, four (3- (3 ' 5 '-two uncles
Butyl -4 '-hydroxy phenyl) propionic acid) pentaerythritol ester, 4,4 '-thiobis (the 6- tert-butyl group -3- methylphenols) or 4,4 '-thio
Double (6- tert-butyl-m-cresols), 4,4 '-thiobis (2- methyl-6-tert-butylphenols) or 4,4 '-thiobis (6- tert-butyl o first
Phenol), 2, the double (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid of 2 '-thiobis (4- methyl-6-tert-butylphenols), hexylene glycol
Ester), 2,2 '-thiobis (3 ,-(3,5- di-tert-butyl-hydroxy phenyl) ethyl propionate), N, double (3,5- bis- uncles of N '-hexamethylene
Butyl-4- hydroxyls hydrocinnamamide), 1,3,5- tri- (the 4- tert-butyl group-3- hydroxyls-2,6- dimethyl benzyls) 1,3,5-triazine-2,4,
6- (1H, 3H, 5H)-triketone, 1,3,5- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) guanamines, 4,6- (1H, 3H, 5H) three
Ketone or isocyanuric acid three (3,5- di-tert-butyl-4-hydroxyl benzyl ester), [β-(3,5- di-t-butyl -4- hydroxy benzenes of isocyanuric acid three
Base) propionyloxy ethyl ester], double [3,3- double (3 '-tert-butyl group -4 '-hydroxy phenyl) butyric acid] glycol esters, 1,1 '-thiobis (2-
Naphthols), double (3,5- di-tert-butyl-4-hydroxyl benzyl) thioethers, 2,5- di-tert-butyl hydroquinones, the tertiary pentyls of 2,5- bis- are to benzene two
Phenol, 3,5- di-tert-butyl-4-hydroxyl benzyls di(2-ethylhexyl)phosphate (18) ester, 3,5- di-tert-butyl-4-hydroxyl benzyls diethyl phosphate, three
One kind in glycol double -3- (3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic ester, hydroquinone dibenzyl ethers.
Phosphite ester kind antioxidant can be enumerated：Triphenyl phosphite, phosphorous acid three (nonyl phenyl ester), phosphorous acid three are different pungent
Ester, triisodecyl phosphite ester, the isodecyl ester of phosphorous acid benzene two, trilauryl trithiophosphite, trilauryl phosphite, phosphorous acid
Three (octadecyl esters), the isodecyl ester of diphosphorous acid pentaerythrite two, diphosphorous acid pentaerythrite distearyl alcohol ester, 4,4 '-fourth fork are double (sub-
Phosphoric acid (3- methyl-6-tert butyl phenyl) two (tridecyl) esters), isooctyl diphenyl phosphite, phosphorous acid benzene di-isooctyl, Asia
Diphenyl octyl phosphate, phosphorous acid hexichol isodecyl ester, dioctyl phosphite, phosphorous acid dilauryl, dimethylphosphite, phosphorous acid
Double 13 esters of two oleyl alcohol esters, didecyl phosphite, dibutyl phosphite, phosphorous acid, phosphorous acid double 14 esters, phosphorous triethylenetetraminehexaacetic acids
Ester, tributyl phosphite, triisopropyl phosphite, the monooctyl ester of phosphorous acid three or phosphorous acid three (2- ethylhexyls), phosphorous acid-benzene are double
One kind in (nonyl benzene) ester, phosphorous acid hexichol nonyl phenyl ester, phosphorous acid three (2,4- di-tert-butyl-phenyl) ester.
It can be enumerated containing sulphur ester antioxidant：Dilauryl thiodipropionate, thio-2 acid 2 stearyl ester or thio
Dipropionic acid two (octadecyl ester), β, β '-thio two butyric acid two (18) ester, thio-2 acid bay octadecyl ester, thio-2 acid two
(13) ester, thio-2 acid two (14) ester are medium.
The plasticizer can be enumerated：Dioctyl phthalate, diisooctyl phthalate, terephthalic acid (TPA) two are pungent
One or more in ester, trioctyl trimellitate (TOTM) or di-n-octyl sebacate.And then preferred cold resistant plasticizer DOS (decanedioic acid
Dioctyl ester) or DOP (dioctyl phthalate) etc..
The fire retardant can be enumerated：It is brominated organic based flame retardant, phosphoric acid based flame retardant, antimony trioxide, magnesium hydroxide, red
Phosphorus etc..
The filler can be enumerated：Silica, aluminum oxide, kaolinite, wollastonite, mica, talcum, clay, sericite,
Magnesium carbonate, magnesium sulfate, calcium oxide, carborundum, antimony trisulphide, artificial gold, copper sulfide, iron sulfide, bismuth sulfide, zinc sulphide, metal
Powder, glass powder, glass flake, montmorillonite, glass microballoon etc..
What the ultra-violet absorber can be enumerated has：2- (2- hydroxy-5-methyl bases phenyl) BTA, 2- (2- hydroxyls-
5- butyl phenyls) BTA, 2- (2- hydroxyl -5- octyl phenyls) BTA, 2- (the 3- tert-butyl group -2- hydroxy-5-methyl base benzene
Base) the enumerate BTA system ultra-violet absorber such as -5- chlorobenzotriazoles, 2- (3,5- bis- tertiary pentyl -2- hydroxy phenyls) BTA；
The benzophenone series ultra-violet absorbers such as ESCALOL 567,2- hydroxyl -4- n-octyl epoxide benzophenone；
2- [4,6- double (2,4- 3,5-dimethylphenyl) -1,3,5-triazines -2- bases] -5- (octyl group epoxide) phenol, 2- (4,6- diphenyl -1,
3,5- triazine -2- bases) the triazine system ultra-violet absorber such as -5- (hexyl epoxide) phenol；P-t-butylphenyl salicylate, salicylic acid
The salicylate such as phenyl ester system ultra-violet absorber etc..
What the antiseptic can be enumerated has：Silver ion class antiseptic, zinc oxide, cupric oxide, ammonium dihydrogen phosphate, carbonic acid
Lithium, anilid class, imidazoles, thiazoles, isothiazolone derivative, quaternary ammonium salt, double croak classes, phenols formic acid, sorbic acid, have
Machine iodine, nitrile, sulphur cyanogen, copper agent, three halogenation allyl compounds, organic nitrogen sulfur compound, chitin, mustard, castor oil, horseradish
Deng.
The fifth aspect of the invention provides a kind of preparation method of PVC composition, at least comprises the following steps：
The polyvinyl chloride resin, superbrnaching end-hydroxy polyester, dibutyl tin laurate of corresponding parts by weight are added to mixed at high speed
In machine, after uniform mixing, 200 DEG C are then placed in again and is kneaded 5~10 minutes in two-roll mill, you can PVC composition is obtained.
The present invention is specifically described below by embodiment.It is necessarily pointed out that, following examples are only used
In the invention will be further described, it is impossible to be interpreted as limiting the scope of the invention, professional and technical personnel in the field
Some the nonessential modifications and adaptations made according to the content of the invention described above, still fall within protection scope of the present invention.
In addition, if without other explanations, it is raw materials used to be all commercially available.
Embodiment 1：
The present embodiment 1 provides a kind of dibutyl tin laurate heat stabilizer, the system of the dibutyl tin laurate
Preparation Method, at least comprises the following steps：
Laurate, dibutyl tin dichloride, ethanol are sequentially added into reactor, wherein, laurate, dichloro dibutyl
Mol ratio 2 between tin, ethanol：1：10, after stirring, sequentially add the catalyst, (sulfydryl third of trimethylolpropane-three
Acid esters), at 40 DEG C, then stirring reaction 30min adds sodium hydroxide solution, the pH value of regulation reaction is 7, and then
At 40 DEG C, stirring reaction 1h after reaction terminates, obtains reaction solution；Then the solvent in reaction solution is distilled out, produced
Thing, after product is washed, is drying to obtain dibutyl tin laurate；
The catalyst is that N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
In the catalyst, weights of the N- (2- aminoethyls) between -3- aminopropyl trimethoxysilanes and mesoporous silicon oxide
Measuring ratio is：1：10；The mesoporous silicon oxide is MCM-41；
Weight ratio between the catalyst, trimethylolpropane-three (mercaptopropionic acid ester) is 100：3；
Weight ratio between the catalyst and laurate is 1：100.
The preparation method of the catalyst, at least comprises the following steps：
In the reactor, solvent 100ml toluene and 10g MCM-41, ultrasonic disperse 10min are added, 1g N- are then added
(2- aminoethyls) -3- aminopropyl trimethoxysilanes, add the triethylamine solution that volumetric concentration is 10%, are flowed back at 100 DEG C
2h is reacted, filtering, ethanol is washed 3 times, be dried to obtain N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes and be modified titanium dioxide
Silicon.
A kind of PVC composition, in parts by weight, at least including following raw material,
100 parts of polyvinyl chloride resin；
1 part of the dibutyl tin laurate of embodiment 1.
The preparation method of the PVC composition, at least comprises the following steps：
The polyvinyl chloride resin of corresponding parts by weight, dibutyl tin laurate are added in high-speed mixer, after uniform mixing,
Then it is placed in 200 DEG C again to knead 5 minutes in two-roll mill, you can obtain PVC composition.
Embodiment 2：
The present embodiment 2 provides a kind of dibutyl tin laurate heat stabilizer, the system of the dibutyl tin laurate
Preparation Method, at least comprises the following steps：
Laurate, dibutyl tin dichloride, ethanol are sequentially added into reactor, wherein, laurate, dichloro dibutyl
Mol ratio 2 between tin, ethanol：1：10, after stirring, sequentially add the catalyst, (sulfydryl third of trimethylolpropane-three
Acid esters), at 40 DEG C, then stirring reaction 30min adds sodium hydroxide solution, the pH value of regulation reaction is 7, and then
At 40 DEG C, stirring reaction 1h after reaction terminates, obtains reaction solution；Then the solvent in reaction solution is distilled out, produced
Thing, after product is washed, is drying to obtain dibutyl tin laurate；
The catalyst is that N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
In the catalyst, weights of the N- (2- aminoethyls) between -3- aminopropyl trimethoxysilanes and mesoporous silicon oxide
Measuring ratio is：3：10；The mesoporous silicon oxide is MCM-41；
Weight ratio between the catalyst, trimethylolpropane-three (mercaptopropionic acid ester) is 100：3；
Weight ratio between the catalyst and laurate is 1：100.
The preparation method of the catalyst, at least comprises the following steps：
In the reactor, solvent 100ml toluene and 10g MCM-41, ultrasonic disperse 10min are added, 1g N- are then added
(2- aminoethyls) -3- aminopropyl trimethoxysilanes, add the triethylamine solution that volumetric concentration is 10%, are flowed back at 100 DEG C
2h is reacted, filtering, ethanol is washed 3 times, be dried to obtain N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes and be modified titanium dioxide
Silicon.
A kind of PVC composition, in parts by weight, at least including following raw material,
100 parts of polyvinyl chloride resin；
1 part of the dibutyl tin laurate of embodiment 2.
A kind of preparation method of PVC composition, at least comprises the following steps：
The polyvinyl chloride resin of corresponding parts by weight, dibutyl tin laurate are added in high-speed mixer, after uniform mixing,
Then it is placed in 200 DEG C again to knead 5 minutes in two-roll mill, you can obtain PVC composition.
Embodiment 3：
The present embodiment 3 provides a kind of dibutyl tin laurate heat stabilizer, the system of the dibutyl tin laurate
Preparation Method, at least comprises the following steps：
Laurate, dibutyl tin dichloride, ethanol are sequentially added into reactor, wherein, laurate, dichloro dibutyl
Mol ratio 2 between tin, ethanol：1：10, after stirring, sequentially add the catalyst, (sulfydryl third of trimethylolpropane-three
Acid esters), at 40 DEG C, then stirring reaction 30min adds sodium hydroxide solution, the pH value of regulation reaction is 7, and then
At 40 DEG C, stirring reaction 1h after reaction terminates, obtains reaction solution；Then the solvent in reaction solution is distilled out, produced
Thing, after product is washed, is drying to obtain dibutyl tin laurate；
The catalyst is that N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
In the catalyst, weights of the N- (2- aminoethyls) between -3- aminopropyl trimethoxysilanes and mesoporous silicon oxide
Measuring ratio is：1：5；The mesoporous silicon oxide is MCM-41；
Weight ratio between the catalyst, trimethylolpropane-three (mercaptopropionic acid ester) is 100：3；
Weight ratio between the catalyst and laurate is 1：100.
The preparation method of the catalyst, at least comprises the following steps：
In the reactor, solvent 100ml toluene and 10g MCM-41, ultrasonic disperse 10min are added, 1g N- are then added
(2- aminoethyls) -3- aminopropyl trimethoxysilanes, add the triethylamine solution that volumetric concentration is 10%, are flowed back at 100 DEG C
2h is reacted, filtering, ethanol is washed 3 times, be dried to obtain N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes and be modified titanium dioxide
Silicon.
A kind of PVC composition, in parts by weight, at least including following raw material,
100 parts of polyvinyl chloride resin；
1 part of the dibutyl tin laurate of embodiment 3.
A kind of preparation method of PVC composition, at least comprises the following steps：
The polyvinyl chloride resin of corresponding parts by weight, dibutyl tin laurate are added in high-speed mixer, after uniform mixing,
Then it is placed in 200 DEG C again to knead 5 minutes in two-roll mill, you can obtain PVC composition.
Embodiment 4：
The present embodiment 4 provides a kind of dibutyl tin laurate heat stabilizer, the system of the dibutyl tin laurate
Preparation Method, at least comprises the following steps：
Laurate, dibutyl tin dichloride, ethanol are sequentially added into reactor, wherein, laurate, dichloro dibutyl
Mol ratio 2 between tin, ethanol：1：10, after stirring, sequentially add the catalyst, (sulfydryl third of trimethylolpropane-three
Acid esters), at 40 DEG C, then stirring reaction 30min adds sodium hydroxide solution, the pH value of regulation reaction is 7, and then
At 40 DEG C, stirring reaction 1h after reaction terminates, obtains reaction solution；Then the solvent in reaction solution is distilled out, produced
Thing, after product is washed, is drying to obtain dibutyl tin laurate；
The catalyst is that dibutyl tin laurate load N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified
Mesoporous silicon oxide.
In the catalyst, weights of the N- (2- aminoethyls) between -3- aminopropyl trimethoxysilanes and mesoporous silicon oxide
Measuring ratio is：1：5；The mesoporous silicon oxide is MCM-41；
Weight ratio between the catalyst, trimethylolpropane-three (mercaptopropionic acid ester) is 100：3；
Weight ratio between the catalyst and laurate is 0.5：100.
The preparation method of the catalyst, at least comprises the following steps：
In the reactor, solvent 100ml toluene and 10g SBA-15, ultrasonic disperse 10min are added, 1g N- are then added
(2- aminoethyls) -3- aminopropyl trimethoxysilanes, add the triethylamine solution that volumetric concentration is 10%, are flowed back at 100 DEG C
2h is reacted, filtering, ethanol is washed 3 times, be dried to obtain N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes and be modified titanium dioxide
Silicon.
By dibutyl tin laurate dissolving in ethanol, it is made into the dibutyl tin laurate that mass fraction is 5% molten
Liquid, then, then addition N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes modification Jie into dibutyl tin laurate solution
Hole silica, is stirred 2 hours at 25 DEG C, stewing process 4 hours, through filtering, washing, dry after obtain di lauric dibutyl
Tin load N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
A kind of PVC composition, in parts by weight, at least including following raw material,
100 parts of polyvinyl chloride resin；
1 part of the dibutyl tin laurate of embodiment 4.
A kind of preparation method of PVC composition, at least comprises the following steps：
The polyvinyl chloride resin of corresponding parts by weight, dibutyl tin laurate are added in high-speed mixer, after uniform mixing,
Then it is placed in 200 DEG C again to knead 5 minutes in two-roll mill, you can obtain PVC composition.
Embodiment 5：
The present embodiment 5 provides a kind of dibutyl tin laurate composite thermal stabilizer, at least including following raw material,
100 parts of dibutyl tin laurate；
3 parts of epoxidized linseed oil；
5 parts of beta-diketon；
The preparation method of the dibutyl tin laurate, at least comprises the following steps：
Laurate, dibutyl tin dichloride, ethanol are sequentially added into reactor, wherein, laurate, dichloro dibutyl
Mol ratio 2 between tin, ethanol：1：10, after stirring, sequentially add the catalyst, (sulfydryl third of trimethylolpropane-three
Acid esters), at 40 DEG C, then stirring reaction 30min adds sodium hydroxide solution, the pH value of regulation reaction is 7, and then
At 40 DEG C, stirring reaction 1h after reaction terminates, obtains reaction solution；Then the solvent in reaction solution is distilled out, produced
Thing, after product is washed, is drying to obtain dibutyl tin laurate；
The catalyst is that dibutyl tin laurate load N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified
Mesoporous silicon oxide.
In the catalyst, weights of the N- (2- aminoethyls) between -3- aminopropyl trimethoxysilanes and mesoporous silicon oxide
Measuring ratio is：1：5；The mesoporous silicon oxide is MCM-41；
Weight ratio between the catalyst, trimethylolpropane-three (mercaptopropionic acid ester) is 100：3；
Weight ratio between the catalyst and laurate is 0.5：100.
The preparation method of the catalyst, at least comprises the following steps：
In the reactor, solvent 100ml toluene and 10g SBA-15, ultrasonic disperse 10min are added, 1g N- are then added
(2- aminoethyls) -3- aminopropyl trimethoxysilanes, add the triethylamine solution that volumetric concentration is 10%, are flowed back at 100 DEG C
2h is reacted, filtering, ethanol is washed 3 times, be dried to obtain N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes and be modified titanium dioxide
Silicon.
By dibutyl tin laurate dissolving in ethanol, it is made into the dibutyl tin laurate that mass fraction is 5% molten
Liquid, then, then addition N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes modification Jie into dibutyl tin laurate solution
Hole silica, is stirred 2 hours at 25 DEG C, stewing process 4 hours, through filtering, washing, dry after obtain di lauric dibutyl
Tin load N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
A kind of PVC composition, in parts by weight, at least including following raw material,
100 parts of polyvinyl chloride resin；
1 part of the dibutyl tin laurate of embodiment 5.
A kind of preparation method of PVC composition, at least comprises the following steps：
The polyvinyl chloride resin of corresponding parts by weight, dibutyl tin laurate are added in high-speed mixer, after uniform mixing,
Then it is placed in 200 DEG C again to knead 5 minutes in two-roll mill, you can obtain PVC composition.
Embodiment 6：
The present embodiment 6 provides a kind of dibutyl tin laurate composite thermal stabilizer, at least including following raw material,
100 parts of dibutyl tin laurate；
3 parts of epoxidized linseed oil；
5 parts of beta-diketon；
The preparation method of the dibutyl tin laurate, at least comprises the following steps：
Laurate, dibutyl tin dichloride, ethanol are sequentially added into reactor, wherein, laurate, dichloro dibutyl
Mol ratio 2 between tin, ethanol：1：10, after stirring, sequentially add the catalyst, (sulfydryl third of trimethylolpropane-three
Acid esters), at 40 DEG C, then stirring reaction 30min adds sodium hydroxide solution, the pH value of regulation reaction is 7, and then
At 40 DEG C, stirring reaction 1h after reaction terminates, obtains reaction solution；Then the solvent in reaction solution is distilled out, produced
Thing, after product is washed, is drying to obtain dibutyl tin laurate；
The catalyst is that dibutyl tin laurate load N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified
Mesoporous silicon oxide.
In the catalyst, weights of the N- (2- aminoethyls) between -3- aminopropyl trimethoxysilanes and mesoporous silicon oxide
Measuring ratio is：1：5；The mesoporous silicon oxide is MCM-41；
Weight ratio between the catalyst, trimethylolpropane-three (mercaptopropionic acid ester) is 100：3；
Weight ratio between the catalyst and laurate is 0.5：100.
The preparation method of the catalyst, at least comprises the following steps：
In the reactor, solvent 100ml toluene and 10g SBA-15, ultrasonic disperse 10min are added, 1g N- are then added
(2- aminoethyls) -3- aminopropyl trimethoxysilanes, add the triethylamine solution that volumetric concentration is 10%, are flowed back at 100 DEG C
2h is reacted, filtering, ethanol is washed 3 times, be dried to obtain N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes and be modified titanium dioxide
Silicon.
By dibutyl tin laurate dissolving in ethanol, it is made into the dibutyl tin laurate that mass fraction is 5% molten
Liquid, then, then addition N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes modification Jie into dibutyl tin laurate solution
Hole silica, is stirred 2 hours at 25 DEG C, stewing process 4 hours, through filtering, washing, dry after obtain di lauric dibutyl
Tin load N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
A kind of PVC composition, in parts by weight, at least including following raw material,
100 parts of polyvinyl chloride resin；
10 parts of superbrnaching end-hydroxy polyester；
1 part of the dibutyl tin laurate of embodiment 6.
A kind of preparation method of PVC composition, at least comprises the following steps：
The polyvinyl chloride resin, superbrnaching end-hydroxy polyester, dibutyl tin laurate of corresponding parts by weight are added to mixed at high speed
In machine, after uniform mixing, 200 DEG C are then placed in again and is kneaded 10 minutes in two-roll mill, you can PVC composition is obtained.
The superbrnaching end-hydroxy polyester is purchased from Wuhan hyperbranched resin Science and Technology Ltd..
Comparative example 1：
The detailed process be the same as Example 1 of comparative example 1, difference is, is added without catalyst.
Comparative example 2：
The detailed process be the same as Example 1 of comparative example 2, difference is, is added without (the mercaptopropionic acid of trimethylolpropane-three
Ester).
Comparative example 3：
The detailed process be the same as Example 1 of comparative example 3, difference is, catalyst is only mesoporous silicon oxide.
Comparative example 4：
The detailed process be the same as Example 1 of comparative example 4, difference is, catalyst is only N- (2- aminoethyls) -3- aminopropyls three
Methoxy silane.
Comparative example 5：
The detailed process be the same as Example 1 of comparative example 5, difference is, by N- (2- aminoethyls) -3- aminopropyl trimethoxy silicon
Alkane is replaced by epoxy silane coupling agent KH560.
Comparative example 6：
The detailed process be the same as Example 1 of comparative example 6, difference is, mesoporous silicon oxide is replaced by into nano silicon,
The nano silicon is purchased from Hangzhou Wanjing New Material Co., Ltd..
Method of testing：
1st, the product in embodiment and comparative example is cut into long a width of 3cm × 2cm, thickness is 1.0mm sample, is put
Enter and static thermal ageing test carried out in 180 ± 1 DEG C of baking ovens, the change of color is observed every 10min, until sample start to occur it is black
The time of point is set to heat-stable time.
2nd, congo red method：Product in embodiment and comparative example is determined according to GB2917-82,180 ± 1 DEG C are placed in
In glycerol bath, determine Congored test paper and start to turn the blue time, be defined as heat-stable time.
3rd, transparency：The thick prints of 1mm are respectively prepared in product in embodiment and comparative example, is tested and marked using transparency
It is accurate：The transparency of GB2410-80 method test sample.
The characterization test of table 1
| Embodiment | Heat-stable time/min | Congo red method/min | Transparency |
| Embodiment 1 | 278 | 230 | 88% |
| Embodiment 2 | 275 | 229 | 89% |
| Embodiment 3 | 282 | 243 | 90% |
| Embodiment 4 | 300 | 255 | 94% |
| Embodiment 5 | 340 | 265 | 95% |
| Embodiment 6 | 380 | 270 | 92% |
| Comparative example 1 | 143 | 125 | 81% |
| Comparative example 2 | 220 | 161 | 78% |
| Comparative example 3 | 184 | 140 | 74% |
| Comparative example 4 | 215 | 172 | 79% |
| Comparative example 5 | 156 | 131 | 80% |
| Comparative example 6 | 240 | 170 | 65% |
From table 1 it follows that the dibutyl tin laurate obtained using the preparation method of the application, when it is added to
In PVC, it can cause PVC composition that there is preferable thermal stability, meanwhile, also with higher whiteness.
As can be seen that adding after catalyst from embodiments herein, the system of dibutyl tin laurate can be caused
The standby time foreshortens to 1~2h by 3~4h, the significant increase combined coefficient of dibutyl tin laurate.
Foregoing example is merely illustrative, some features of the feature for explaining the disclosure.Appended claim
The scope as wide as possible for requiring to be contemplated that is intended to, and embodiments as presented herein is only according to all possible embodiment
Combination selection embodiment explanation.Therefore, the purpose of applicant is appended claim not by the explanation present invention
Feature example selectional restriction.And the progress in science and technology by formed language performance it is inaccurate due to and not
The possible equivalent or son being presently considered are replaced, and these changes should also be interpreted by appended in the conceived case
Claim is covered.
Claims (10)
1. a kind of preparation method of dibutyl tin laurate, it is characterised in that at least comprise the following steps：
Laurate, dibutyl tin dichloride, ethanol are sequentially added into reactor, wherein, laurate, dichloro dibutyl tin, second
Mol ratio 2 between alcohol：1：10, after stirring, catalyst, trimethylolpropane-three (mercaptopropionic acid ester) are sequentially added,
At 40 DEG C, then 30~60min of stirring reaction adds sodium hydroxide solution, the pH value of regulation reaction is 7, and is then existed
At 40 DEG C, 1~3h of stirring reaction after reaction terminates, obtains reaction solution；Then the solvent in reaction solution is distilled out, produced
Thing, after product is washed, is drying to obtain dibutyl tin laurate；The catalyst is N- (2- aminoethyls) -3- ammonia third
Base trimethoxy silane is modified mesoporous silicon oxide.
2. the preparation method of dibutyl tin laurate as claimed in claim 1, it is characterised in that in the catalyst, N-
The weight ratio of (2- aminoethyls) between -3- aminopropyl trimethoxysilanes and mesoporous silicon oxide is：(1~3)：10.
3. the preparation method of dibutyl tin laurate as claimed in claim 1 or 2, it is characterised in that the mesoporous dioxy
SiClx is selected from：Any one or a few mixing in MCM-41, MCM-48, MCM-50, SBA-15, SBA-16.
4. the preparation method of dibutyl tin laurate as claimed in claim 3, it is characterised in that the catalyst is February
Dilaurylate load N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified mesoporous silicon oxide.
5. the preparation method of dibutyl tin laurate as claimed in claim 4, it is characterised in that the fourth of tin dilaurate two
The weight ratio that Ji Xi and N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are modified between mesoporous silicon oxide is：1：50.
6. the preparation method of dibutyl tin laurate as claimed in claim 1, it is characterised in that the catalyst, three hydroxyls
Weight ratio between methylpropane-three (mercaptopropionic acid ester) is 100：3.
7. the dibutyl tin laurate that the preparation method of the dibutyl tin laurate as described in claim 1~6 is obtained exists
Heat stabilizer, catalyst, drier, the application of dye field.
8. a kind of dibutyl tin laurate composite thermal stabilizer, it is characterised in that at least including following raw material,
100 parts of dibutyl tin laurate；
1~10 part of epoxidized linseed oil；
5 parts of beta-diketon；
The preparation method of the dibutyl tin laurate is as follows：
Laurate, dibutyl tin dichloride, ethanol are sequentially added into reactor, wherein, laurate, dichloro dibutyl tin, second
Mol ratio 2 between alcohol：1：10, after stirring, catalyst, trimethylolpropane-three (mercaptopropionic acid ester) are sequentially added,
At 40 DEG C, then 30~60min of stirring reaction adds sodium hydroxide solution, the pH value of regulation reaction is 7, and is then existed
At 40 DEG C, 1~3h of stirring reaction after reaction terminates, obtains reaction solution；Then the solvent in reaction solution is distilled out, produced
Thing, after product is washed, is drying to obtain dibutyl tin laurate；The catalyst is N- (2- aminoethyls) -3- ammonia third
Base trimethoxy silane is modified mesoporous silicon oxide.
9. a kind of PVC composition, it is characterised in that in parts by weight, at least including following raw material,
100 parts of polyvinyl chloride resin；
1~10 part of superbrnaching end-hydroxy polyester；
1~3 part of dibutyl tin laurate composite thermal stabilizer described in claim 8.
10. the preparation method of the PVC composition described in claim 9, it is characterised in that at least comprise the following steps：
The polyvinyl chloride resin, superbrnaching end-hydroxy polyester, dibutyl tin laurate of corresponding parts by weight are added to high-speed mixer
In, after uniform mixing, 200 DEG C are then placed in again and is kneaded 5~10 minutes in two-roll mill, you can PVC composition is obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710366937.4A CN107033184B (en) | 2017-05-23 | 2017-05-23 | A kind of preparation method and its product of dibutyl tin dilaurate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710366937.4A CN107033184B (en) | 2017-05-23 | 2017-05-23 | A kind of preparation method and its product of dibutyl tin dilaurate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107033184A true CN107033184A (en) | 2017-08-11 |
| CN107033184B CN107033184B (en) | 2019-03-22 |
Family
ID=59539772
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710366937.4A Active CN107033184B (en) | 2017-05-23 | 2017-05-23 | A kind of preparation method and its product of dibutyl tin dilaurate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107033184B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109294758A (en) * | 2018-08-31 | 2019-02-01 | 浙江帝恒实业有限公司 | A kind of new-energy automobile cleaning agent and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516544A (en) * | 2011-11-23 | 2012-06-27 | 湖北新蓝天新材料股份有限公司 | Method for preparing dibutyltin dilaurate catalyst |
| CN102838631A (en) * | 2012-09-21 | 2012-12-26 | 沧州威达聚氨酯高科股份有限公司 | Synthesis method of dibutyltin dilaurate |
| CN104672276A (en) * | 2015-02-11 | 2015-06-03 | 江苏鑫露化工新材料有限公司 | Synthetic method for preparing dibutyltin dilaurate |
-
2017
- 2017-05-23 CN CN201710366937.4A patent/CN107033184B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516544A (en) * | 2011-11-23 | 2012-06-27 | 湖北新蓝天新材料股份有限公司 | Method for preparing dibutyltin dilaurate catalyst |
| CN102838631A (en) * | 2012-09-21 | 2012-12-26 | 沧州威达聚氨酯高科股份有限公司 | Synthesis method of dibutyltin dilaurate |
| CN104672276A (en) * | 2015-02-11 | 2015-06-03 | 江苏鑫露化工新材料有限公司 | Synthetic method for preparing dibutyltin dilaurate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109294758A (en) * | 2018-08-31 | 2019-02-01 | 浙江帝恒实业有限公司 | A kind of new-energy automobile cleaning agent and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107033184B (en) | 2019-03-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107099104B (en) | Magnalium hydrotalcite composite thermal stabilizer and preparation method thereof, application | |
| CN102746593B (en) | A kind of Nitrile rubber insulation flat cable material and preparation method thereof | |
| CN108102213B (en) | Flame-retardant polypropylene composition and preparation method and application thereof | |
| CN105418901B (en) | High temperature resistance polyester resin used for powder coating of low TGIC consumptions and preparation method thereof | |
| EP3121229A1 (en) | Vinyl chloride resin composition for powder molding, vinyl chloride resin molded article, and laminate | |
| CN107216549A (en) | A kind of antistatic weather-resistance flame-retardant electric instrument shell of high intensity and preparation method thereof | |
| CN106823229A (en) | Efficient and environment-friendly type fire retardant extinguisher and preparation method thereof | |
| CN107556531A (en) | A kind of novel environment friendly stabilizer and preparation method thereof | |
| CN104356565A (en) | Aluminophosphate molecular sieve flame retardant and preparation method thereof | |
| EP3081592A1 (en) | Vinyl chloride resin composition, vinyl chloride resin molded article, and laminate | |
| CN103928172B (en) | Fire retardant crosslinked polyethylene insulated power cable | |
| CN107033184A (en) | The preparation method and its product of a kind of dibutyl tin laurate | |
| CN106977669A (en) | Nuclear-shell structure type ACR resins and preparation method thereof | |
| CN103865196A (en) | Compound rare-earth calcium zinc heat stabilizer as well as preparation method and use method thereof | |
| CN102875980B (en) | Preparation method of heat-resistant oxygen-resistant polyester film | |
| CN109438673B (en) | Low-hydroxyl phosphorus-containing epoxy resin, composition for copper-clad plate and preparation method of composition | |
| CN104725823A (en) | Low-temperature-resistant flame-retardant PC (polycarbonate) composite material and preparation method thereof | |
| CN101735481A (en) | Organic calcium-zinc soap lye stabilizing agent | |
| CN109776780A (en) | A kind of phosphor-containing flame-proof PTT and its preparation method and application | |
| CN104231212A (en) | Conductive PU sole material and manufacturing method thereof | |
| CN104672837A (en) | Low-temperature-resistant chemicals-resistant PC composite material and preparation method thereof | |
| CN106867109A (en) | A kind of low VOC PP composite materials and preparation method thereof | |
| CN103928159B (en) | fireproof power cable | |
| CN107141643B (en) | A kind of barium-zinc liquid heat stabilizer and preparation method thereof, application | |
| CN107033183A (en) | The preparation technology and its product of Methyl stannum mercaptide, application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210819 Address after: 226200 Hezuo Shihai Town, Qidong City, Nantong City, Jiangsu Province Patentee after: Qidong Qiangqiang Trade Co.,Ltd. Address before: 226200 Binjiang fine chemical industry park, Qidong Economic Development Zone, Nantong City, Jiangsu Province Patentee before: NANTONG ADVANCE CHEMICALS Co.,Ltd. |