CN110003523A - A kind of polyester lubricant and preparation method thereof - Google Patents
A kind of polyester lubricant and preparation method thereof Download PDFInfo
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- CN110003523A CN110003523A CN201910335351.0A CN201910335351A CN110003523A CN 110003523 A CN110003523 A CN 110003523A CN 201910335351 A CN201910335351 A CN 201910335351A CN 110003523 A CN110003523 A CN 110003523A
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- reaction system
- temperature
- polyester
- polyester lubricant
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
- C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Lubricants (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The present invention provides a kind of polyester lubricants and preparation method thereof.Wherein the preparation method includes the following steps: under the protection of protective gas, and stearic acid, pentaerythrite, activator, antioxidant are added to heat in a reaction vessel and melted；Control system temperature adds promotor after being kept for 5-6 hours at 180-190 DEG C；System temperature is controlled at 190-200 DEG C, and system temperature is reduced after being kept for temperature 1-2 hours to 150-160 DEG C of discharging to get the polyester lubricant of the present invention.Present invention utilizes efficient activator and promotor, the efficiency and degree of acid and alcohol reaction in system are improved, to improve the thermal stability of product polyester lubricant.The features such as compared with the polyester wax of traditional handicraft preparation, products of the present invention is high with whiteness, color value is low, by-product is few, with high purity, and anti-yellowing property and resistance to precipitation are had excellent performance in use.
Description
Technical field
The present invention relates to a kind of high molecular material higher aliphatic acid polyol ester series lubricant agents, especially, therein one
Kind polyester lubricant and preparation method thereof, is preferably applied to use in PVC transparent sheet material, but be not limited to.
Background technique
It is known that with pentaerythritol stearate (Pentaerythrityl tetrastearate, abbreviation PETS) for representative
Polyester wax lubricant be one of most important processing aid of high molecular material.Wherein PETS has good heat steady at high temperature
The plastics of partially crystallizable are had fabulous nucleation, can be used for by qualitative and low volatility, good demoulding and mobile performance
Bright product.Due to PETS thermal stability outstanding, it is made to can be used for the process of such system, degraded without worrying,
And it can significantly improve transparency and surface smoothness, have a wide range of applications in all kinds of engineering plastics fields.
And with the continuous expansion of high molecular material application field, higher and higher want also proposed to the performance of polyester wax
It asks.The especially easy precipitation of polyester wax and easy xanthochromia performance has seriously affected it in PVC transparent sheet material and other are transparent
Material etc. requires material transparent degree relatively high application field.
Specifically, wherein polyester wax xanthochromia and easily precipitation performance refer mainly in terms of two: first aspect refers to polyester wax
During the preparation process, since production technology is improper and the factors such as raw material, and the polyester wax of original white is caused to easily become
Yellow.The second aspect refers to polyester wax since unreacted is complete, and the extent of reaction is lower, causes to be easy to be precipitated in use
And jaundice, and then influence the appearance of final products.The raising of polyester wax color inhibition and precipitation property is that current production and user grind
Study carefully most eager one of solve the problems, such as.Easily it is precipitated and the yellowing application for having seriously affected polyester wax in terms of transparent composite.
Currently, being mainly enterprising from preparation process about improving polyester wax color inhibition and the research of performance being precipitated and explores
Row, document (Lu the synthesis dayization science and technology .2004 of Fu Tingjin pentaerythritol stearate, the 1st phase: 61-62) and patent (Shen
Please numbers 201610264101.9: a kind of preparation method of pentaerythritol tetraoctyl stearate) give it is some palliative
Method.
Therefore, it is necessory to develop a kind of novel polyester lubricant and preparation method thereof, to overcome in the prior art
Defect.
Summary of the invention
One aspect of the present invention is to provide a kind of polyester lubricant, utilizes efficient activator and promotor, mention
Reaction efficiency and degree in high raw material between acid and alcohol, effectively raise the thermostabilization of polyester lubricant described in product
Property, to be easily precipitated and the performance of xanthochromia fundamentally solving existing polyester wax.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of polyester lubricant prepares raw material including following parts by weight:
90 ~ 120 parts of C18 stearic acid；
13-15 parts of pentaerythrite；
0.5-2 parts of activator；
1-5 parts of promotor；And
0.1-0.5 parts of antioxidant.
Further, in different embodiments, wherein the C18 stearic acid is saturation C18 stearic acid.For example, industry
Known product type is the combination of one of AS1801, AS1840, AS1865 and AS1895 or 2 kinds or more quantity.
Further, in different embodiments, wherein the pentaerythrite is monopentaerythritol.
Further, in different embodiments, wherein the antioxidant packages include antioxidant 1010, irgasfos 168 and boron
One of hydrofining is several.
Further, in different embodiments, wherein the activator and promotor, can be both selections industry
The trade names product known.For example, trade names are the activator product of DZHA-05, the promotor that trade names are HRX is produced
Product, but be not limited to.
It is a further aspect of the present invention to provide a kind of preparation sides for being used to prepare the polyester lubricant of the present invention
Method, comprising the following steps:
Step S1, the C18 stearic acid of 90-120 parts by weight, the pentaerythrite of 13-15 parts by weight, 0.5-2 parts by weight are taken
Activator and the antioxidant of 0.1-0.5 parts by weight be put into a reaction vessel, these raw materials are in the reaction vessel
Constitute a reaction system；
Step S2, the reaction system is placed under the protection of protective gas and is heated up to the reaction system, and is right simultaneously
It is stirred, wherein keeping temperature 4-6h when the temperature of reaction system is increased to 180-190 DEG C；
Step S3,1-5 parts by weight promotor is taken to be added in the reaction system, after 190-200 DEG C of maintenance system temperature
Continue 1.5-3h；
Step S4, the polyester profit of the present invention can be obtained in discharging when temperature of reaction system being reduced to 150-160 DEG C
Lubrication prescription.
Further, in different embodiments, wherein in step S1, the reaction vessel used is with blender, temperature
Spend the four-hole boiling flask of meter.
Further, in different embodiments, wherein in step S1, the stirring to the reaction system is with 260-
What the revolving speed of 360r/min carried out.Specifically, can be 280r/min, 300r/min, 320r/min etc., can with the need and
It is fixed, and be not limited.
Further, in different embodiments, wherein in step S1, the reaction vessel can be placed in the oil of temperature programmed control
In bath, guarantee reaction system in the reaction vessel in the next steps by way of heating oil bath combination temperature programmed control
Temperature control.
Further, in different embodiments, wherein in step S2, the protective gas used is nitrogen or inert gas
Or the common protective gas of other industries, specifically can with the need depending on, and be not limited.
Compared with the existing technology, the beneficial effects of the present invention are: a kind of polyester lubricant of the present invention, passes through and divide
Son design is effectively increased reaction efficiency between pentaerythrite and stearic acid and anti-using efficient activator and promotor
Degree is answered, to improve the saponification number of the two product polyester wax on molecular structure, and then effectively improves the resistance to of product polyester wax
Xanthochromia performance and precipitation performance.
Further, compared with the polyester wax of traditional handicraft preparation, the polyester lubricant preparation side of the present invention
The product of method preparation has many advantages, such as that whiteness is high, color value is low, by-product is few, with high purity, while also having resistance in use
The features such as performance and excellent anti-yellowing property is precipitated, is a kind of preparation method for being suitable for industrialized production polyester lubricant.
Specific embodiment
Below with reference to embodiment, a kind of technical solution of polyester lubricant of the present invention and preparation method thereof is made
It is described in further detail.
Wherein in the present invention, all raw material used be it is conventional use of, can be bought from market.In this hair
It in bright, is refered in particular to Ru non-, all amounts, percentage, part are parts by weight unit.
For ease of understanding, below by with the preparation method of polyester lubricant involved in each embodiment come to each embodiment into
Row description explanation.
Embodiment 1
100 grams of AS1801,13 grams of pentaerythrites, 0.5 gram of activator, 0.1 gram of antioxidant is taken to be put into blender, thermometer
A reaction system is formed in four-hole boiling flask and in bottle, and the four-hole boiling flask is placed in the oil bath of temperature programmed control；
The reaction system is placed in nitrogen protection and opens that the blender starts to stir and opening program temperature regulating device adds
Hot oil bath reads the temperature reading, when the temperature of reaction system is raised to close to 180 DEG C, controls the reaction system
Temperature at 180 DEG C or so, keep 5 hours；
It weighs 1 gram of promotor to be added in the reaction system, after promotor is added, controls the temperature of the reaction system
At 190 DEG C or so, kept for 2 hours；
It reduces the temperature of reaction system and is produced to 160 DEG C with bottom discharge to get polyester lubricant embodiment 1 of the present invention
Product.
Embodiment 2
Take 100 grams of AS1801,15 grams of pentaerythrites, 2 grams of activators, 0.5 gram of antioxidant be put into blender, thermometer four
A reaction system is formed in mouth flask and in bottle, the four-hole boiling flask is placed in the oil bath of temperature programmed control；
The reaction system is placed in nitrogen protection and opens that the blender starts to stir and opening program temperature regulating device adds
Hot oil bath reads the temperature reading, after the temperature of reaction system is raised to 180 DEG C, controls the temperature of the reaction system
Degree is kept for 6 hours at 190 DEG C or so；
It weighs 5 grams of promotors to be added in the reaction system, after promotor is added, controls the temperature of the reaction system
At 200 DEG C or so, kept for 2 hours；
It reduces the temperature of reaction system and is produced to 160 DEG C with bottom discharge to get polyester lubricant embodiment 2 of the present invention
Product.
Embodiment 3
100 grams of AS1840,13 grams of pentaerythrites, 0.5 gram of activator, 0.1 gram of antioxidant is taken to be put into blender, thermometer
A reaction system is formed in four-hole boiling flask and in bottle, and the four-hole boiling flask is placed in the oil bath of temperature programmed control；
The reaction system is placed in nitrogen protection and opens that the blender starts to stir and opening program temperature regulating device adds
Hot oil bath reads the temperature reading, when the temperature of reaction system is raised to close to 180 DEG C, controls the reaction system
Temperature at 180 DEG C or so, keep 5 hours；
It weighs 1 gram of promotor to be added in the reaction system, after promotor is added, controls the temperature of the reaction system
At 190 DEG C or so, kept for 2 hours；
It reduces the temperature of reaction system and is produced to 160 DEG C with bottom discharge to get polyester lubricant embodiment 3 of the present invention
Product.
Embodiment 4
Take 100 grams of AS1840,15 grams of pentaerythrites, 2 grams of activators, 0.5 gram of antioxidant be put into blender, thermometer four
A reaction system is formed in mouth flask and in bottle, the four-hole boiling flask is placed in the oil bath of temperature programmed control；
The reaction system is placed in nitrogen protection and opens that the blender starts to stir and opening program temperature regulating device adds
Hot oil bath reads the temperature reading, after the temperature of reaction system is raised to 180 DEG C, controls the temperature of the reaction system
Degree is kept for 6 hours at 190 DEG C or so；
It weighs 5 grams of promotors to be added in the reaction system, after promotor is added, controls the temperature of the reaction system
At 200 DEG C or so, kept for 2 hours；
It reduces the temperature of reaction system and is produced to 160 DEG C with bottom discharge to get polyester lubricant embodiment 4 of the present invention
Product.
Embodiment 5
100 grams of AS1865,13 grams of pentaerythrites, 0.5 gram of activator, 0.1 gram of antioxidant is taken to be put into blender, thermometer
A reaction system is formed in four-hole boiling flask and in bottle, and the four-hole boiling flask is placed in the oil bath of temperature programmed control；
The reaction system is placed in nitrogen protection and opens that the blender starts to stir and opening program temperature regulating device adds
Hot oil bath reads the temperature reading, when the temperature of reaction system is raised to close to 180 DEG C, controls the reaction system
Temperature at 180 DEG C or so, keep 5 hours；
It weighs 1 gram of promotor to be added in the reaction system, after promotor is added, controls the temperature of the reaction system
At 190 DEG C or so, kept for 2 hours；
It reduces the temperature of reaction system and is produced to 160 DEG C with bottom discharge to get polyester lubricant embodiment 5 of the present invention
Product.
Embodiment 6
Take 100 grams of AS1865,15 grams of pentaerythrites, 2 grams of activators, 0.5 gram of antioxidant be put into blender, thermometer four
A reaction system is formed in mouth flask and in bottle, the four-hole boiling flask is placed in the oil bath of temperature programmed control；
The reaction system is placed in nitrogen protection and opens that the blender starts to stir and opening program temperature regulating device adds
Hot oil bath reads the temperature reading, after the temperature of reaction system is raised to 180 DEG C, controls the temperature of the reaction system
Degree is kept for 6 hours at 190 DEG C or so；
It weighs 5 grams of promotors to be added in the reaction system, after promotor is added, controls the temperature of the reaction system
At 200 DEG C or so, kept for 2 hours；
It reduces the temperature of reaction system and is produced to 160 DEG C with bottom discharge to get polyester lubricant embodiment 6 of the present invention
Product.
Embodiment 7
100 grams of AS1895,13 grams of pentaerythrites, 0.5 gram of activator, 0.1 gram of antioxidant is taken to be put into blender, thermometer
A reaction system is formed in four-hole boiling flask and in bottle, and the four-hole boiling flask is placed in the oil bath of temperature programmed control；
The reaction system is placed in nitrogen protection and opens that the blender starts to stir and opening program temperature regulating device adds
Hot oil bath reads the temperature reading, when the temperature of reaction system is raised to close to 180 DEG C, controls the reaction system
Temperature at 180 DEG C or so, keep 5 hours；
It weighs 1 gram of promotor to be added in the reaction system, after promotor is added, controls the temperature of the reaction system
At 190 DEG C or so, kept for 2 hours；
It reduces the temperature of reaction system and is produced to 160 DEG C with bottom discharge to get polyester lubricant embodiment 7 of the present invention
Product.
Embodiment 8
Take 100 grams of AS1895,15 grams of pentaerythrites, 2 grams of activators, 0.5 gram of antioxidant be put into blender, thermometer four
A reaction system is formed in mouth flask and in bottle, the four-hole boiling flask is placed in the oil bath of temperature programmed control；
The reaction system is placed in nitrogen protection and opens that the blender starts to stir and opening program temperature regulating device adds
Hot oil bath reads the temperature reading, after the temperature of reaction system is raised to 180 DEG C, controls the temperature of the reaction system
Degree is kept for 6 hours at 190 DEG C or so；
It weighs 5 grams of promotors to be added in the reaction system, after promotor is added, controls the temperature of the reaction system
At 200 DEG C or so, kept for 2 hours；
It reduces the temperature of reaction system and is produced to 160 DEG C with bottom discharge to get polyester lubricant embodiment 8 of the present invention
Product.
Embodiment 9
100 grams of AS1865,13 grams of pentaerythrites, 0.5 gram of activator, 0.1 gram of antioxidant is taken to be put into blender, thermometer
A reaction system is formed in four-hole boiling flask and in bottle, and the four-hole boiling flask is placed in the oil bath of temperature programmed control；
The reaction system is placed in nitrogen protection and opens that the blender starts to stir and opening program temperature regulating device adds
Hot oil bath reads the temperature reading, when the temperature of reaction system is raised to close to 180 DEG C, controls the reaction system
Temperature at 180 DEG C or so, keep 6 hours；
It weighs 3.5 grams of promotors to be added in the reaction system, after promotor is added, controls the temperature of the reaction system
Degree is kept for 2 hours at 190 DEG C or so；
It reduces the temperature of reaction system and is produced to 160 DEG C with bottom discharge to get polyester lubricant embodiment 9 of the present invention
Product.
Embodiment 10
100 grams of AS1865,13 grams of pentaerythrites, 0.5 gram of activator, 0.1 gram of antioxidant is taken to be put into blender, thermometer
A reaction system is formed in four-hole boiling flask and in bottle, and the four-hole boiling flask is placed in the oil bath of temperature programmed control；
The reaction system is placed in nitrogen protection and opens that the blender starts to stir and opening program temperature regulating device adds
Hot oil bath reads the temperature reading, after the temperature of reaction system is raised to 180 DEG C, controls the temperature of the reaction system
Degree is kept for 6 hours at 190 DEG C or so；
It weighs 3.5 grams of promotors to be added in the reaction system, after promotor is added, controls the temperature of the reaction system
Degree is kept for 2 hours at 200 DEG C or so；
It reduces the temperature of reaction system and is produced to 160 DEG C with bottom discharge to get polyester lubricant embodiment 10 of the present invention
Product.
Further, by above is referred to each embodiment obtain polyester lubricant embodiment 1-10 product, carry out resistance to Huang
Become test.It mainly tests its yellowness index YI, and specific practice is the heat for embodiment 1-10 sample polyester wax being put into 300 DEG C
In ageing oven, its YI value is tested after placing 10 minutes and 25 minutes respectively.Then with commercial polyesters wax (PETS) yellowness index pair
Than specific test result see the table below 1.
Table 1: the sample polyester wax that embodiment 1-10 is obtained is compared with commercial polyesters wax (PETS) yellowness index YI
| Number | YI(room temperature) | YI(300 DEG C * 10 minutes) | YI(300 DEG C * 25 minutes) |
| Commercial polyesters wax (PETS) | 4.1 | 5.5 | 10.2 |
| Embodiment 1 | 3.5 | 4.6 | 6.2 |
| Embodiment 2 | 3.1 | 4.6 | 5.7 |
| Embodiment 3 | 3.3 | 4.3 | 5.9 |
| Embodiment 4 | 3.0 | 4.0 | 5.7 |
| Embodiment 5 | 2.3 | 4.8 | 5.9 |
| Embodiment 6 | 2.4 | 4.1 | 5.8 |
| Embodiment 7 | 2.6 | 4.6 | 5.7 |
| Embodiment 8 | 2.8 | 4.4 | 6.0 |
| Embodiment 9 | 2.5 | 4.0 | 5.8 |
| Embodiment 10 | 2.0 | 3.6 | 4.8 |
According to above-mentioned yellowness index YI data, the sample polyester wax of embodiment 1-10 of the present invention can be clearly found out,
It is better than commercial product in anti-yellowing property.
Resistance to precipitation test is carried out to embodiment 1-10 product of the present invention, to add embodiment 1-10 product respectively
Enter into PVC, in double rod testing machines, 190 DEG C of temperature, carries out plasticizing hacking 4 minutes, 7 minutes, 10 minutes, 15 minutes, 18 points
Its surface is observed after clock respectively, situation is precipitated.According to subsequent photo comparison, it is believed that be equally better than commercial product.
In summary test result, embodiment 1-10 product of the present invention is in anti-yellowing property and resistance to precipitation performance
It is better than commercial polyesters wax (PETS), has reached goal of the invention.
Technical scope of the invention is not limited solely to the content in above description, and those skilled in the art can not take off
Under the premise of from technical thought of the invention, many variations and modifications are carried out to above-described embodiment, and these deformations and modification should all
When within the scope of the present invention.
Claims (10)
1. a kind of polyester lubricant；It is characterised in that it includes following parts by weight prepare raw material:
2. polyester lubricant according to claim 1；It is characterized in that, wherein the C18 stearic acid is that saturation C18 is stearic
Acid.
3. polyester lubricant according to claim 1；It is characterized in that, wherein the C18 stearic acid includes 2 kinds or more
Quantity C18 stearic acid combination not of the same race.
4. polyester lubricant according to claim 1；It is characterized in that, wherein the pentaerythrite is monopentaerythritol.
5. polyester lubricant according to claim 1；It is characterized in that, wherein the antioxidant packages include antioxidant 1010,
One of irgasfos 168 and potassium borohydride are several.
6. a kind of preparation method for being used to prepare polyester lubricant according to claim 1；It is characterised in that it includes following step
It is rapid:
Step S1, the C18 stearic acid of 90-120 parts by weight, the pentaerythrite of 13-15 parts by weight, 0.5-2 parts by weight are taken
Activator and the antioxidant of 0.1-0.5 parts by weight be put into a reaction vessel, these raw materials are in the reaction vessel
Constitute a reaction system；
Step S2, the reaction system is placed under the protection of protective gas and starts to heat up to the reaction system, and is same
When it is stirred, wherein when the temperature of reaction system is increased to 180-190 DEG C, keep temperature 4-6h；
Step S3,1-5 parts by weight promotor is taken to be added in the reaction system, after 190-200 DEG C of maintenance system temperature
Continue 1.5-3h；
Step S4, the discharging when temperature of reaction system being reduced to 150-160 DEG C, can be obtained according to claim 1
Polyester lubricant.
7. polyester lubricant preparation method according to claim 6；It is characterized in that, what is used is anti-wherein in step S1
Answering container is the four-hole boiling flask with blender, thermometer.
8. polyester lubricant preparation method according to claim 6；It is characterized in that, wherein in step S1, to described anti-
The stirring for answering system is carried out with the revolving speed of 260-360r/min.
9. polyester lubricant preparation method according to claim 6；It is characterized in that, wherein in step S1, the reaction
Container can be placed in the oil bath of temperature programmed control, be guaranteed in the reaction vessel by way of heating oil bath combination temperature programmed control
The temperature control of reaction system in the next steps.
10. polyester lubricant preparation method according to claim 6；It is characterized in that, wherein in step S2, the guarantor that uses
Protecting gas is nitrogen or inert gas.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103880669A (en) * | 2012-12-24 | 2014-06-25 | 青岛帅王油脂化学有限公司 | Pentaerythritol stearate preparation method |
| CN104529767A (en) * | 2014-12-11 | 2015-04-22 | 青岛佰众化工技术有限公司 | Synthetic method of pour point depressant pentaerythritol stearate |
| CN108976143A (en) * | 2018-08-17 | 2018-12-11 | 苏州联胜化学有限公司 | Color inhibition amide waxe and preparation method thereof |
| CN109666182A (en) * | 2018-11-28 | 2019-04-23 | 苏州联胜化学有限公司 | A kind of brightener and preparation method thereof |
-
2019
- 2019-04-24 CN CN201910335351.0A patent/CN110003523A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103880669A (en) * | 2012-12-24 | 2014-06-25 | 青岛帅王油脂化学有限公司 | Pentaerythritol stearate preparation method |
| CN104529767A (en) * | 2014-12-11 | 2015-04-22 | 青岛佰众化工技术有限公司 | Synthetic method of pour point depressant pentaerythritol stearate |
| CN108976143A (en) * | 2018-08-17 | 2018-12-11 | 苏州联胜化学有限公司 | Color inhibition amide waxe and preparation method thereof |
| CN109666182A (en) * | 2018-11-28 | 2019-04-23 | 苏州联胜化学有限公司 | A kind of brightener and preparation method thereof |
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