CN105372156B - A kind of method of test evaluation PVC STABILIZERS/LUBRICANTS resin lubrication performance - Google Patents
A kind of method of test evaluation PVC STABILIZERS/LUBRICANTS resin lubrication performance Download PDFInfo
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Abstract
The present invention relates to a kind of methods that PVC STABILIZERS/LUBRICANTS resin lubrication performance is evaluated in system testing, belong to technical field of chemical industry；The specific steps are：（1）Corvic, heat stabilizer are mediated uniformly in mixing machine, are configured to mixing material；（2）Corvic, heat stabilizer and lubricant are mediated uniformly in mixing machine, are configured to mixing material；（3）It is kneaded mixing material with the mixer of torque rheometer, rheological curve is recorded, fusion time is read by rheological curve；（4）When being used alone by Integrated comparative lubricant to the degree of PVC plastic time effects and with high-performance main effect resin external lubricant and type with effect（Additive effect, synergistic effect or antagonistic effect）And it is strong and weak, to evaluate the resin lubrication performance of lubricant.This method can not only differentiate the resin lubrication function of lubricant but also can distinguish its performance height, and simple possible, as a result accurately and reliably.
Description
Technical field
The present invention relates to a kind of test evaluation methods of PVC STABILIZERS/LUBRICANTS resin lubrication performance, and in particular to Yi Zhongyong
Torque rheometer measures lubricant and is used alone and with high-performance main effect resin external lubricant and with the influence to the PVC plastic time
Method to evaluate its resin lubrication performance, belongs to technical field of chemical industry.
Background technology
Polyvinyl chloride（PVC）It is one of five big general-purpose plastics, there is intensity height, can be plasticized, is corrosion-resistant, is fire retardant, insulating properties
The advantages that good, transparent high, product tool has been widely used.But PVC is since polarity is stronger, each hierarchical structure unit
（Including each level particle and molecule）And they all have stronger interaction and friction between process equipment metal surface
Power, therefore that there are melt viscosities is high, material cutting frictional heat is big and melt is serious to the adherency of process equipment metal surface etc.
Processability problems.These processability problems and to thermally labile superposition lead to the extremely difficult thermoplastic processings of PVC.It therefore, be to PVC
Thermoplastic processing is carried out, in addition to it must use heat stabilizer, while it is necessary that with lubricator.Currently, in the market have aliphatic acid,
The type of lubricant such as metallic soap, carboxylate, fatty acid amide, fatty alcohol and chloroflo are alternative.Unfortunately, due to these profits
Also not very fully, until current, in PVC processing, the application of lubricant is largely for the characteristic of lubrication prescription and the understanding of action principle
On be still empirical.It is investigated according to the system of the author, it is multi-functional that this, which is mainly due to PVC lubricants, has just been recognized at present
For knowing, including metal lubrication（Commonly referred to as demould）And resin lubrication, and resin lubrication include it is interior lubrication, it is outer lubrication and
The outer lubrication of auxiliary, and these functions can effectively be distinguished and evaluate its strong and weak test evaluation method by not yet establishing at present.
In PVC lubricants, some kinds can be dissolved in PVC melts to PVC in weakening melt at the process conditions
The effect of inter-molecular attraction, lubricating action in this effect, that is, resin, lubrication in lubricant, that is, resin with this function
Agent；Some kinds at the process conditions do not dissolve in PVC melts but can PVC particle surfaces sprawl thus with reduce PVC particles
Between attraction effect, the outer lubricating action of this effect, that is, main effect resin, outside lubricant, that is, main effect resin with this function
Lubricant；And some kinds both unobvious with lubricating action in resin or unobvious with the outer lubricating action of main effect resin, but
But have the function of that collaboration enhancing main effect resin external lubricant performance, the outer lubricating action of this effect, that is, assisted resin have this
The lubricant of one function, that is, assisted resin external lubricant.
Obviously, test evaluation method is established to differentiate the different practical resin lubrications having the function of of PVC lubricants and area
Divide its performance strong and weak, there is basic meaning for research, the development and application of PVC lubricants.Unfortunately, so far there is not yet
Related report.
Invention content
The purpose of the present invention overcomes the shortcomings of the prior art, and provides a kind of independent with torque rheometer measurement lubricant
Using and with high-performance main effect resin external lubricant and with the influence to the PVC plastic time, to differentiate its resin lubrication function simultaneously
The method for distinguishing its performance height.
To achieve the goals above, the technical solution adopted in the present invention is：
A kind of test evaluation method of PVC STABILIZERS/LUBRICANTS resin lubrication performance, includes the following steps：
（1）It is prepared by blank mixing material：Corvic, heat stabilizer are mediated uniformly in mixing machine, are configured to match
Batch mixing；
（2）It is prepared by mixing material containing lubricant：Corvic, heat stabilizer and lubricant are mediated in mixing machine
It is even, it is configured to mixing material；
（3）Mixing material fusion time measures：It is kneaded mixing material with the mixer of torque rheometer, records rheological curve, by
Rheological curve reads fusion time；
（4）Lubricant resin lubrication performance evaluation：The mixing material containing lubricant and blank measured more under the same conditions
The fusion time of mixing material differentiates the resin lubrication function of lubricant and distinguishes its performance power as follows：
Can extend the fusion time of PVC when exclusive use and with high-performance main effect resin external lubricant and used time pair
The influence of PVC plastic time has additive effect（I.e. the performance of two components be more than each be used alone performance it
With）Person is main effect resin external lubricant, and it is higher to extend PVC plastic time more notable then performance when exclusive use；
2. when being used alone on the fusion time of PVC influence unobvious but with high-performance main effect resin external lubricant and used time
Influence to the PVC plastic time has synergistic effect（I.e. the performance of two components is more than the performance that each is used alone
The sum of）Person is assisted resin external lubricant, with the more strong then performance of synergistic effect of high-performance main effect resin external lubricant more
It is high；
Be used alone on the fusion time of PVC influence unobvious but with high-performance main effect resin external lubricant and used time pair
The influence of PVC plastic time has antagonistic effect（I.e. the performance of two components be less than each be used alone performance it
With）Person is resin in-lubricant, higher with the more strong then performance of antagonistic effect of high-performance main effect resin external lubricant.
Described to be kneaded mixing material with torque rheometer mixer, condition is 160 ~ 220 DEG C of mixer temperature, rotor speed 10
~ 80rpm, preferably 180 ~ 200 DEG C of mixer temperature, 30 ~ 60rpm of rotor speed；The high-performance main effect resin external lubricant
Paraffin wax lubricants are synthesized for High performance polyolefin wax lubricant, high-performance oil wax lubricant or high-performance.
The advantageous effect of the present invention compared with the existing technology is：
Establish by with torque rheometer measure lubricant be used alone and with high-performance main effect resin external lubricant simultaneously
With the influence to the PVC plastic time, and to the degree and and high-performance of PVC plastic time effects when its exclusive use of Integrated comparative
Main effect resin external lubricant and type with effect（Additive effect, synergistic effect or antagonistic effect）And it is strong and weak, to differentiate it
Resin lubrication function can distinguish the PVC lubricant resin lubrication performance system test evaluation methods of its performance height again.
Figure of description
Several typical resins lubricants of Fig. 1 are used alone and with A-C 617A and with the influence to the PVC plastic time, from
It is upper and lower curve corresponds to lubricant：Nothing, 0.8phrGMS, 0.8phrHSt, 5phrGMS, 5phrHSt；
Fig. 2 torque rheological curve of the PVC mixing materials containing GMS and HSt, Δ without lubricant and respectivelyt f= t f (containing profit
Lubrication prescription mixing material)- t f (blank mixing material), from top to bottom curve correspond to lubricant (A+B)：(MgSt2+ A-C 617A)、
(CaSt2+ A-C 617A), (A-C617 A+ A-C617 A), (A-C 6+ A-C617A), (without+A-C617A), (GMS+ A-
C617A), (HSt+ A-C617A), corresponding total dosage/phr：0.8, 0.8, 0.8, 0.8, 0.8ω(B), 0.8, 0.8。
Specific implementation mode
The present invention is described in further details below by embodiment, these embodiments are only used for illustrating the present invention, and
It does not limit the scope of the invention.
Embodiment 1
A kind of method of test evaluation PVC STABILIZERS/LUBRICANTS resin lubrication performance, includes the following steps：
（1）It is prepared by blank mixing material：By 100phr（Mass parts）Polyvinyl chloride resin, 1phr thiol methyl tin heat stabilizers are in height
It is mediated uniformly in fast Universalpulverizer, is configured to mixing material；
（2）It is prepared by mixing material containing lubricant：By 100phr（Mass parts）Polyvinyl chloride resin, 1phr thiol methyl tin heat stabilizers
Respectively with A-C 617A and A-C the 6A mixtures of 0.8phr polyethylene waxes A-C 617A, A-C 6A and different proportion in high speed ten thousand
It can be mediated uniformly in pulverizer, be configured to mixing material；
（3）Mixing material fusion time measures：With the mixer of torque rheometer in 190 DEG C of temperature, rotor speed 45rpm items
Blank and mixing material containing lubricant are kneaded under part respectively, rheological curve is recorded, fusion time is read by rheological curve；
（4）Lubricant resin lubrication performance evaluation：The mixing material containing lubricant and blank measured more under the same conditions
The fusion time of mixing material differentiates the resin lubrication function of lubricant and distinguishes its performance power as follows：
Can extend the fusion time of PVC when exclusive use and with polyethylene wax A-C 617A and the used time is to PVC plastic
It is main effect resin external lubricant that additive effect person, which is presented, in the influence of time, when exclusive use extend the PVC plastic time more it is notable then
Performance is higher；
2. influencing unobvious to the fusion time of PVC when being used alone but with polyethylene wax A-C 617A and the used time is to PVC
Synergistic effect person is presented in the influence of fusion time is assisted resin external lubricant, and effect is cooperateed with polyethylene wax A-C 617A
Then performance is higher by Ying Yueqiang；
Be used alone influences unobvious but with polyethylene wax A-C617A and the used time is to PVC plastic to the fusion time of PVC
It is resin in-lubricant that antagonistic effect person, which is presented, in the influence of time, with the antagonistic effect of polyethylene wax A-C 617A more it is strong then
Performance is higher.
Test result is shown in Fig. 1 and table 1.
Embodiment 2
A kind of method of test evaluation PVC STABILIZERS/LUBRICANTS resin lubrication performance, it is substantially the same manner as Example 1, difference
It is in and is changed in the preparation of mixing material containing lubricant：
By 100phr（Mass parts）Polyvinyl chloride resin, 1phr thiol methyls tin heat stabilizer respectively with 0.8phr polyethylene waxes A-C
617A, calcium stearate（CaSt2）And the A-C 617A and CaSt of different proportion2Mixture is mediated in high speed Universal pulverizer
It is even, it is configured to mixing material.
Test result is shown in Fig. 1 and table 1.
Embodiment 3
A kind of method of test evaluation PVC STABILIZERS/LUBRICANTS resin lubrication performance, it is substantially the same manner as Example 1, difference
It is in and is changed in the preparation of mixing material containing lubricant：
By 100phr（Mass parts）Polyvinyl chloride resin, 1phr thiol methyls tin heat stabilizer respectively with 0.8phr polyethylene waxes A-C
617A, magnesium stearate（MgSt2）And the A-C 617A and MgSt of different proportion2Mixture is mediated in high speed Universal pulverizer
It is even, it is configured to mixing material.
Test result is shown in Fig. 1 and table 1.
Embodiment 4
A kind of method of test evaluation PVC STABILIZERS/LUBRICANTS resin lubrication performance, it is substantially the same manner as Example 1, difference
It is in and is changed in the preparation of mixing material containing lubricant：
By 100phr（Mass parts）Polyvinyl chloride resin, 1phr thiol methyls tin heat stabilizer respectively with 0.8phr polyethylene waxes A-
C 617A, glycerin monostearate（GMS）And A-C 617A and the GMS mixtures of different proportion are pinched in high speed Universal pulverizer
It closes uniformly, is configured to mixing material.
Test result is shown in Fig. 1 and table 1.
Embodiment 5
A kind of method of test evaluation PVC STABILIZERS/LUBRICANTS resin lubrication performance, it is substantially the same manner as Example 1, difference
It is in and is changed in the preparation of mixing material containing lubricant：
By 100phr（Mass parts）Polyvinyl chloride resin, 1phr thiol methyls tin heat stabilizer respectively with 0.8phr polyethylene waxes A-
C 617A, stearic acid（HSt）And A-C 617A and the HSt mixtures of different proportion are mediated uniformly in high speed Universal pulverizer,
It is configured to mixing material.
Test result is shown in Fig. 1 and table 1.
Comparative example
By comparing the method for greasy property in temperature of charge and torque evaluation PVC lubricant resins, include the following steps：
（1）It is prepared by blank mixing material：By 100phr（Mass parts）Polyvinyl chloride resin, 1phr thiol methyl tin heat stabilizers are in height
It is mediated uniformly in fast Universalpulverizer, is configured to mixing material；
（2）It is prepared by mixing material containing lubricant：By 100phr（Mass parts）Polyvinyl chloride resin, 1phr thiol methyl tin heat stabilizers
It is mediated in high speed Universal pulverizer uniformly with certain phr lubricants, is configured to mixing material；
（3）Mixing material rheological curve measures：With the mixer of torque rheometer in 190 DEG C of temperature, rotor speed 45rpm items
Blank and mixing material containing lubricant are kneaded under part respectively, records rheological curve；
（4）Evaluation of Lubrication in lubricant resin：By comparing under the same conditions be kneaded mixing material containing lubricant with
When blank mixing material the temperature of material and torque evaluation, if mixing material containing lubricant compared with blank mixing material, temperature of charge
Decline with torque, then lubricant has lubricating function in resin, and the degree that temperature of charge and torque decline is bigger, then in resin
Greasy property is higher.
The blank mixing material that is measured by comparative example method contains 0.8phr, 5.0phrGMS mixing material and contains respectively respectively
0.8phr, 5.0phrHSt mixing material rheological curve are shown in Fig. 2.
Polyethylene wax A-C 6A and A-C 617A are that the famous brand high-performance main effect resin that Honeywell Inc. produces lubricates outside
Agent, wherein A-C 617A are the innovative products of A-C 6A, have the outer greasy property of higher main effect resin.
CaSt2And MgSt2It is common assisted resin external lubricant, and in contrast, MgSt2Performance higher.CaSt2With
MgSt2It is main effect resin external lubricant-PVC particle interfaces to be stablized by interfacial adsorption as surfactant by play master
Imitate the outer lubricating action of resin.Why MgSt2With than CaSt2The outer greasy property of higher assisted resin is because of the two knot
Structure is similar, Mg2+With Ca2+Though charge is identical but the former radius smaller, therefore in contrast, MgSt2Polar head polarity is stronger, surface
Activity is also just stronger, can more effectively stablize main effect resin external lubricant-PVC particle interfaces.
GMS and HSt is common resin in-lubricant, and in contrast, HSt performance highers.Resin in-lubricant is because can
Weaken PVC inter-molecular attractions in melt, therefore not only have the function of promoting PVC plastic, while it is viscous also to reduce PVC melts
Degree.Resin in-lubricant can reduce PVC melt viscosities and show in torque rheology characteristic, can exactly reduce temperature of charge（Yin Mo
Heat is wiped to reduce）And torque.Obviously, it reduces temperature of charge and torque degree is bigger, illustrate greasy property in the resin of lubricant
It is higher.
From Figure 2 it can be seen that compared with the blank PVC mixing materials without lubricant, the material of the PVC mixing materials containing GMS and HSt
Temperature and torque decline, and show that GMS and HSt have lubricating action in resin really.And it can also be seen that by Fig. 1 and pass through measurement
The individually torque rheology characteristic of the PVC mixing materials containing GMS and HSt, when dosage is in normal ranges（0.8phr）When, it can not effective district
Divide its performance difference；Performance is effectively distinguished, dosage must be increased to unconventional range.Compare dosage be 5phr containing GMS and
The torque rheology characteristic of the PVC mixing materials of HSt, it may be determined that HSt has greasy property in resin more higher than GMS.
Speculated according to performance characteristics as described above, if measuring above-mentioned typical resins lubricant with the method for the present invention, is answered
This obtains following result：
(1) fusion time that can extend PVC is used alone in polyethylene wax A-C617A and A-C6A, with high-performance main effect tree
Fat external lubricant and with there are additive effects, and in contrast, the ability that A-C 617A extend the PVC plastic time is better than A-C
6A。
(2)CaSt2And MgSt2Be used alone influences unobvious to the fusion time of PVC, moistens with outside high-performance main effect resin
Lubrication prescription and with having synergistic effect, and in contrast, MgSt2It is better than with the synergistic effect of high-performance main effect resin external lubricant
CaSt2。
(3) GMS and HSt is used alone influences unobvious to the fusion time of PVC, with high-performance main effect resin external lubricant
The effect that creates antagonism is used in combination（The PVC plastic time is caused to shorten）, and in contrast, HSt is lubricated with outside high-performance main effect resin
The antagonistic effect of agent is better than GMS.
With 1 ~ embodiment of embodiment, 3 method measure several typical resins lubricants be used alone and with high-performance main effect resin
External lubricant A-C 617A and with to the PVC plastic time（t f）Influence the results are shown in Figure 1.
According to the test result of Fig. 1, several typical resins lubricants and A-C 617A by it is best and with than（Mass ratio 1:4,
With most strong and use effect）It is used in combination and 1 is shown in Table to the specific effect of PVC plastic time effects.
Δt f= t f(mixing material containing lubricant)- t f(blank mixing material)
By Fig. 1 and table 1, it can be seen that, test result just matches with above-mentioned according to speculating made by performance characteristics.This is just
Demonstrate the feasibility of the method for the present invention.
In addition, as previously mentioned, by measuring influence of the resin in-lubricant to temperature of charge and torque with torque rheometer,
Though can also differentiate its function, its performance is effectively distinguished, dosage must be but increased to unconventional range.However, by Fig. 1 and
If table 1 as it can be seen that carry out test evaluation with the method for the present invention, its function just can have not only been differentiated under the conditions of conventional amount used but also effective
Distinguish its performance.Usually it can more preferably reflect subject in reality based on the test evaluation result obtained under the conditions of conventional amount used
Effect under processing conditions, it is believed that new method is more scientific.
Why component B will use " high-performance " main effect resin external lubricant, because outside using " high-performance " main effect resin
Lubricant can generate strong and with effect, be conducive to effectively distinguish the resin lubrication function of different PVC lubricants and distinguish its performance
It is strong and weak.
Claims (3)
1. a kind of method of test evaluation PVC STABILIZERS/LUBRICANTS resin lubrication performance, which is characterized in that include the following steps：
（1）It is prepared by blank mixing material：Corvic, heat stabilizer are mediated uniformly in mixing machine, are configured to mixing material；
（2）It is prepared by mixing material containing lubricant：Corvic, heat stabilizer and lubricant are mediated uniformly in mixing machine,
It is configured to mixing material；
（3）Mixing material fusion time measures：It is kneaded mixing material with torque rheometer mixer, records rheological curve, by rheology song
Line reads fusion time；
（4）Lubricant resin lubrication performance evaluation：Mixing material containing lubricant and the blank compounding measured more under the same conditions
The fusion time of material differentiates the resin lubrication function of lubricant and distinguishes its performance power as follows：
The fusion time of PVC can be extended when 1. being used alone and with high-performance main effect resin external lubricant and used time to PVC plastic
Changing the influence of time, additive effect person is presented is main effect resin external lubricant, and it is more notable to extend the PVC plastic time when exclusive use
Then performance is higher；
2. when being used alone on the fusion time of PVC influence unobvious but with high-performance main effect resin external lubricant and used time pair
It is assisted resin external lubricant that synergistic effect person, which is presented, in the influence of PVC plastic time, simultaneously with high-performance main effect resin external lubricant
The more strong then performance of synergistic effect is higher；
3. be used alone influences unobvious but with high-performance main effect resin external lubricant and the used time is to PVC to the fusion time of PVC
It is resin in-lubricant, the confrontation with high-performance main effect resin external lubricant that antagonistic effect person, which is presented, in the influence of fusion time
The more strong then performance of effect is higher；
Step（3）It is kneaded mixing material with torque rheometer mixer, condition is 160 DEG C ~ 220 DEG C of mixer temperature, rotor speed
10 rpm ~80rpm。
2. a kind of method of test evaluation PVC STABILIZERS/LUBRICANTS resin lubrication performance according to claim 1, feature
It is：Step（3）It is kneaded mixing material with torque rheometer mixer, condition is 180 DEG C ~ 200 DEG C of mixer temperature, rotor speed
30 rpm ~60rpm。
3. a kind of method of test evaluation PVC STABILIZERS/LUBRICANTS resin lubrication performance according to claim 1, feature
It is：The high-performance main effect resin external lubricant is High performance polyolefin wax lubricant, high-performance oil wax lubricant or height
Performance synthesizes paraffin wax lubricants.
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| CN106093354B (en) * | 2016-07-05 | 2018-12-21 | 广东工业大学 | A kind of method of lubricant plate-out in test evaluation Hard PVC |
| CN109227993A (en) * | 2018-07-17 | 2019-01-18 | 广东工业大学 | A method of PVC STABILIZERS/LUBRICANTS pressure analysis adherency in cleaning torque rheometer mixer |
| CN109054237B (en) * | 2018-07-17 | 2021-02-19 | 广东工业大学 | Method for cleaning adhesion of polyvinyl chloride melt in mixer of torque rheometer |
| CN109054251A (en) * | 2018-08-10 | 2018-12-21 | 广东工业大学 | A method of PVC STABILIZERS/LUBRICANTS pressure analysis adherency in cleaning torque rheometer mixer |
| CN109135113A (en) * | 2018-08-10 | 2019-01-04 | 广东工业大学 | A method of polyvinyl chloride melt adherency in cleaning torque rheometer mixer |
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| 新型PVC润滑剂的制备及其性能研究;张慧蓉;《中国优秀硕士论文全文数据库 工程科技I辑》;20130315(第3期);第9页最后一段，第12页第3段，第23页第2段和表2-3，第30页第2、3段，第31页图2-10和表2-6 * |
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