CN107286332A - A kind of pre-accelerated thixotropic Anchor Agent resin and preparation method thereof - Google Patents
A kind of pre-accelerated thixotropic Anchor Agent resin and preparation method thereof Download PDFInfo
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- CN107286332A CN107286332A CN201710655699.9A CN201710655699A CN107286332A CN 107286332 A CN107286332 A CN 107286332A CN 201710655699 A CN201710655699 A CN 201710655699A CN 107286332 A CN107286332 A CN 107286332A
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- anchor agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/676—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The present invention provides a kind of pre-accelerated thixotropic Anchor Agent resin and preparation method thereof, and Anchor Agent resin is made up of the raw material according to following weight：30~35 parts of PET chemical fibres waste material, 25~30 parts of fumaric acid, 4~6 parts of cis-butenedioic anhydride, 0.75~1.25 part of benzoic acid, 2~3 parts of ethylene glycol, 20~30 parts of diethylene glycol (DEG), 3~4 parts of propane diols, 40~50 parts of styrene, 0.5~0.6 part of dimethylaniline, 0.5~0.6 part of accelerator, 0.15~0.3 part of white carbon, 0.01~0.05 part of quinhydrones, 0.01~0.05 part of naphthoquinones, 0.01~0.02 part of hydroquinones.The appropriate white carbon of pre-add, makes resin have thixotropy in resin, it is ensured that the stability of resin-bonded mastic during follow-up Anchor Agent, improves product quality, simplifies production process, reduces production cost.The p-phenyl's polyester resin for carrying out strand regulation production using a variety of alcohol and a variety of acid has relatively low production cost, relatively low acid number and higher solidification intensity, fully meets quality requirement of the resin anchoring agent production to resin.
Description
Technical field
The present invention relates to chemical field, a kind of specifically pre-accelerated thixotropic Anchor Agent resin and preparation method thereof.
Background technology
Anchor Agent resin is the main material for producing resin anchoring agent, and it is formulated unique, it is desirable to which not only compression strength is high, also
Want curing rate fast, 80 degrees Celsius of material after being mixed with various stone flours and accelerator is thermally-stabilised to be more than more than 20 hours, and tool
There is thixotropic property, while requiring that cost is relatively low.
The resin of production resin anchoring agent is mainly versatility resin now, and cured strength is not high, and stability is poor, gel
Time is long, and production blending process is complicated, and cost is higher.
The content of the invention
It is mainly versatility resin the invention aims to the resin for solving to produce resin anchoring agent in the prior art,
Cured strength is not high, and stability is poor, and gel time is long, and production blending process is complicated, and there is provided one kind for the higher defect of cost
Pre-accelerated thixotropic Anchor Agent resin and preparation method thereof solves the above problems.
To achieve these goals, technical scheme is as follows：
A kind of pre-accelerated thixotropic Anchor Agent resin, it is constituted according to the raw material of following weight：PET chemical fibre waste materials
30~35 parts, 25~30 parts of fumaric acid, 4~6 parts of cis-butenedioic anhydride, 0.75~1.25 part of benzoic acid, 2~3 parts of ethylene glycol, diethylene glycol (DEG) 20~
30 parts, 3~4 parts of propane diols, 40~50 parts of styrene, 0.5~0.6 part of dimethylaniline, 0.5~0.6 part of accelerator, white carbon
0.15~0.3 part, 0.01~0.05 part of quinhydrones, 0.01~0.05 part of naphthoquinones, 0.01~0.02 part of hydroquinones.
It is preferred that, Anchor Agent resin also includes 0.03~0.05 part of auxiliary material
It is preferred that, Anchor Agent resin is constituted according to the raw material of following weight：32.5 parts of PET chemical fibres waste material, rich horse
27.5 parts of acid, 5 parts of cis-butenedioic anhydride, 1 part of benzoic acid, 2.5 parts of ethylene glycol, 25 parts of diethylene glycol (DEG), 3.5 parts of propane diols, 45 parts of styrene, diformazan
0.55 part of base aniline, 0.55 part of accelerator, 0.225 part of white carbon, 0.025 part of quinhydrones, 0.025 part of naphthoquinones, hydroquinones 0.015
Part, auxiliary material 0.04.
The present invention also provides a kind of preparation method of pre-accelerated thixotropic Anchor Agent resin, comprises the following steps：
1) once feed intake
Diethylene glycol (DEG) is first put into reactor in proportion, then ethylene glycol add catalyst, stirring is opened after finishing to be made to urge
Agent is uniformly dispersed；After catalyst is uniform, stop stirring, then put into whole PET chemical fibre waste materials；Feed intake and start to add after finishing
Heat is heated up and stirred, when material temperature is raised to 230 DEG C, and 160 DEG C are cooled to after insulation 3.5h；
2) secondary batching
Propane diols, cis-butenedioic anhydride, fumaric acid, benzoic acid and part hydroquinones are put into reactor, two throwings terminate follow-up
It is continuous to be warming up to 170 DEG C or so water outlets, one hour follow-up temperature of continuing rising is kept, programming rate is controlled at 3 hours or so to 190 DEG C, then
With being raised within 2 hours 210 DEG C, be incubated 1 hour, sampling detecting acid number in 50 ± 2mg KOH/g, vacuumize surveyed after 1 hour acid number 30 ±
2mg KOH/g, that is, be made polyester semi-finished product stand-by；
3) cool latting drown
Polyester semi-product material in question response kettle cools to 185 DEG C and places remaining hydroquinones, then cools to 145
DEG C, turn material into the thinning vessel for the styrene for having squeezed into 1,4-naphthoquinone, turn during material in thinning vessel temperature control 85 DEG C with
It is interior；Turn to cool to less than 65 DEG C after material terminates, then add white carbon, dimethylaniline, the accelerator of ormal weight, stirring makes it
Mixing is abundant, and resin viscosity as defined in is then adjusted with styrene.
It is preferred that, in secondary batching, 0.006 part of hydroquinones is first put into, remaining 0.009 part of hydroquinones is in cooling latting drown
During put into.
The present invention compared with prior art, has the advantages that：
The use of PET reclaimed materials is that raw material produces resin, waste material is recycled, production cost is reduced, environment is reduced
Pollution.Dimethylaniline and accelerator are previously added in resin, pre-accelerated type resin is produced, made in follow-up Anchor Agent life
Accelerator need not be added during production again, the quality conformance of Anchor Agent is improved and simplifies production process.In resin
The appropriate white carbon of pre-add, makes resin have thixotropy, it is ensured that the stability of resin-bonded mastic during follow-up Anchor Agent, improves product matter
Amount, simplifies production process, reduces production cost.
The p-phenyl's polyester resin for carrying out strand regulation production using a variety of alcohol and a variety of acid has relatively low be produced into
This, relatively low acid number and higher solidification intensity fully meet quality requirement of the resin anchoring agent production to resin, and simplify
The production process of Anchor Agent, reduce further Anchor Agent production cost and quality-control cost.
Embodiment
To make to have a better understanding and awareness to architectural feature of the invention and the effect reached, to preferably
Embodiment is described in detail, and is described as follows：
Embodiment 1
A kind of pre-accelerated thixotropic Anchor Agent resin, it is constituted according to the raw material of following weight：PET chemical fibre waste materials
30~35 parts, 25~30 parts of fumaric acid, 4~6 parts of cis-butenedioic anhydride, 0.75~1.25 part of benzoic acid, 2~3 parts of ethylene glycol, diethylene glycol (DEG) 20~
30 parts, it is 3~4 parts of propane diols, 40~50 parts of styrene, 0.5~0.6 part of dimethylaniline, 0.5~0.6 part of efficient accelerator, white
0.15~0.3 part of carbon black, 0.01~0.05 part of quinhydrones, 0.01~0.05 part of naphthoquinones, 0.01~0.02 part of hydroquinones, other are auxiliary
0.03~0.05 part of material.
When Anchor Agent resin is constituted according to the raw material of following weight, performance is optimal：32.5 parts of PET chemical fibres waste material,
27.5 parts of fumaric acid, 5 parts of cis-butenedioic anhydride, 1 part of benzoic acid, 2.5 parts of ethylene glycol, 25 parts of diethylene glycol (DEG), 3.5 parts of propane diols, 45 parts of styrene,
0.55 part of dimethylaniline, 0.55 part of accelerator, 0.225 part of white carbon, 0.025 part of quinhydrones, 0.025 part of naphthoquinones, hydroquinones
0.015 part, auxiliary material 0.04.
Embodiment 2
A kind of preparation method of pre-accelerated thixotropic Anchor Agent resin, comprises the following steps：
Step 1. first time feeds intake
Diethylene glycol (DEG) is first put into reactor in proportion, then ethylene glycol add catalyst, stirring is opened after finishing to be made to urge
Agent is uniformly dispersed.Stop stirring, then put into whole PET；Feed intake and finish, open hot-oil circulation valve heat temperature raising.If one
Secondary property is thrown endless, side heating plus can also be fed intake, as temperature raises the dissolving of material, untill finishing.With material temperature by
Step rise, until major part PET is degraded in kettle, stirring formally starts stirring when can bear resistance completely.Heat up later stage note
Meaning control evaporates a temperature, because PET material reaction water is seldom, to avoid alcohol from being lost in as far as possible, evaporate a temperature less than 105 degree.Work as material
When temperature rise is to 230 degree, 3.5 hours are incubated, 160 DEG C are then cooled to.
Step 2. secondary batching
Put into propane diols, cis-butenedioic anhydride, fumaric acid, benzoic acid, 0.006 part of hydroquinones, two throw and terminate follow-up continuous to be warming up to 170
DEG C or so water outlet, keep one hour follow-up temperature of continuing rising, control programming rate be raised at 3 hours or so to 190 DEG C, then with 2 hours
210 DEG C, 1 hour is incubated, sampling detecting acid number vacuumizes survey acid number 30 ± 2mg KOH/g after 1 hour, i.e., in 50 ± 2mg KOH/g
Polyester semi-finished product are made stand-by.
Step 3. cooling latting drown
Polyester semi-product material in reactor, cools to and remaining hydroquinones is placed after 185 DEG C, then cool to 145
DEG C, turn material into the thinning vessel for the styrene for having squeezed into 1,4-naphthoquinone, turn during material in thinning vessel temperature control 85 DEG C with
It is interior.Turn to cool to less than 65 DEG C after material terminates, then add the white carbon of ormal weight, dimethylaniline, efficient accelerator, stirring
More than 1 hour, make its mixing abundant, resin viscosity as defined in is then adjusted with styrene.
Using Anchor Agent resin all technical such as table 1 made from above-mentioned preparation method：
Table 1
Pass through Anchor Agent Resin A made from the above method and Anchor Agent resin B performance comparison such as table 2 made from conventional method
It is shown：
Table 2
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and that described in above-described embodiment and specification is the present invention
Principle, various changes and modifications of the present invention are possible without departing from the spirit and scope of the present invention, these change and
Improvement is both fallen within the range of claimed invention.The protection domain of application claims by appended claims and its
Equivalent is defined.
Claims (5)
1. a kind of pre-accelerated thixotropic Anchor Agent resin, it is characterised in that：It is constituted according to the raw material of following weight：
30~35 parts of PET chemical fibres waste material, 25~30 parts of fumaric acid, 4~6 parts of cis-butenedioic anhydride, 0.75~1.25 part of benzoic acid, ethylene glycol 2~3
Part, 20~30 parts of diethylene glycol (DEG), 3~4 parts of propane diols, 40~50 parts of styrene, 0.5~0.6 part of dimethylaniline, accelerator 0.5
~0.6 part, 0.15~0.3 part of white carbon, 0.01~0.05 part of quinhydrones, 0.01~0.05 part of naphthoquinones, hydroquinones 0.01~
0.02 part.
2. a kind of pre-accelerated thixotropic Anchor Agent resin according to claim 1, it is characterised in that：Anchor Agent resin is also wrapped
Include 0.03~0.05 part of auxiliary material.
3. a kind of pre-accelerated thixotropic Anchor Agent resin according to claim 1, it is characterised in that：Anchor Agent resin according to
The raw material composition of following weight：32.5 parts of PET chemical fibres waste material, 27.5 parts of fumaric acid, 5 parts of cis-butenedioic anhydride, 1 part of benzoic acid, second
It is 2.5 parts of glycol, 25 parts of diethylene glycol (DEG), 3.5 parts of propane diols, 45 parts of styrene, 0.55 part of dimethylaniline, 0.55 part of accelerator, white
0.225 part of carbon black, 0.025 part of quinhydrones, 0.025 part of naphthoquinones, 0.015 part of hydroquinones, auxiliary material 0.04.
4. a kind of preparation method of pre-accelerated thixotropic Anchor Agent resin as described in claims 1 to 3 is any, its feature exists
In：Comprise the following steps：
1) once feed intake
Diethylene glycol (DEG) is first put into reactor in proportion, then ethylene glycol add catalyst, stirring is opened after finishing makes catalyst
It is uniformly dispersed；After catalyst is uniform, stop stirring, then put into whole PET chemical fibre waste materials；Feed intake and liter is begun to warm up after finishing
Temperature is simultaneously stirred, when material temperature is raised to 230 DEG C, and 160 DEG C are cooled to after insulation 3.5h；
2) secondary batching
Propane diols, cis-butenedioic anhydride, fumaric acid, benzoic acid and part hydroquinones are put into reactor, two throwings terminate follow-up of continuing rising
Temperature keeps one hour follow-up temperature of continuing rising to 170 DEG C or so water outlets, and control programming rate is small at 3 hours or so to 190 DEG C, then with 2
When be raised to 210 DEG C, be incubated 1 hour, sampling detecting acid number vacuumizes and 30 ± 2mg of acid number is surveyed after 1 hour in 50 ± 2mg KOH/g
KOH/g, that is, be made polyester semi-finished product stand-by；
3) cool latting drown
Polyester semi-product material in question response kettle cools to 185 DEG C and places remaining hydroquinones, then cools to 145 DEG C, to
Turn material in the thinning vessel for the styrene for having squeezed into 1,4-naphthoquinone, turn during material in thinning vessel temperature control within 85 DEG C；Turn
Material cools to less than 65 DEG C after terminating, and then adds white carbon, dimethylaniline, the accelerator of ormal weight, and stirring mixes it
Fully, resin viscosity as defined in is then adjusted with styrene.
5. the preparation method of pre-accelerated thixotropic Anchor Agent resin according to claim 4, it is characterised in that：Secondary batching
In, 0.006 part of hydroquinones is first put into, remaining 0.009 part of hydroquinones is put into during cooling latting drown.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710655699.9A CN107286332A (en) | 2017-08-03 | 2017-08-03 | A kind of pre-accelerated thixotropic Anchor Agent resin and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710655699.9A CN107286332A (en) | 2017-08-03 | 2017-08-03 | A kind of pre-accelerated thixotropic Anchor Agent resin and preparation method thereof |
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| CN107286332A true CN107286332A (en) | 2017-10-24 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110105554A (en) * | 2019-05-07 | 2019-08-09 | 淮南舜天合成材料有限责任公司 | The dedicated unsaturated polyester resin synthetic method of naphthalene method FMA Anchor Agent and technique |
| CN111233372A (en) * | 2020-01-07 | 2020-06-05 | 美亚高新材料股份有限公司 | Comprehensive utilization method of large parameters of coal gangue in anchoring agent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104163890A (en) * | 2013-12-11 | 2014-11-26 | 淮北金久新型材料有限公司 | Resin anchoring agent and preparation method thereof |
| CN106496535A (en) * | 2016-10-25 | 2017-03-15 | 美亚高新材料股份有限公司 | Special unsaturated polyester resin of a kind of recycled PET type Anchor Agent and preparation method thereof |
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2017
- 2017-08-03 CN CN201710655699.9A patent/CN107286332A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163890A (en) * | 2013-12-11 | 2014-11-26 | 淮北金久新型材料有限公司 | Resin anchoring agent and preparation method thereof |
| CN106496535A (en) * | 2016-10-25 | 2017-03-15 | 美亚高新材料股份有限公司 | Special unsaturated polyester resin of a kind of recycled PET type Anchor Agent and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 吴培熙等: "《塑料制品生产工艺手册》", 31 July 1996, 化学工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110105554A (en) * | 2019-05-07 | 2019-08-09 | 淮南舜天合成材料有限责任公司 | The dedicated unsaturated polyester resin synthetic method of naphthalene method FMA Anchor Agent and technique |
| CN111233372A (en) * | 2020-01-07 | 2020-06-05 | 美亚高新材料股份有限公司 | Comprehensive utilization method of large parameters of coal gangue in anchoring agent |
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Application publication date: 20171024 |