Method for predicting roll sticking property of PVC paste resin

Abstract

The invention belongs to the technical field of PVC paste resin detection, and particularly relates to a method for predicting the roll sticking property of PVC paste resin. According to the method, a rotational rheometer is adopted to carry out frequency scanning on PVC paste resin at a fixed amplitude and a constant temperature to obtain a loss modulus-frequency relation curve and an energy storage modulus-frequency relation curve, and then a complex viscosity-angular frequency relation curve is drawn; and predicting the roll sticking property of the PVC paste resin sample through the angular frequency value of the lowest point of the complex viscosity-angular frequency relation curve. The method is suitable for analyzing and predicting the roll sticking property of the PVC paste resin on line, so that the time-consuming and complicated process caused by adjusting the processing temperature after roll sticking is avoided. The method is simple, reliable, wide in application range and suitable for popularization and application in industrial production.

Description

Technical Field

[0001] The invention belongs to the technical field of PVC paste resin detection, and in particular relates to a method for predicting roller stickiness of PVC paste resin. Background Art

[0002] Polyvinyl chloride (PVC) paste resin is also called PVC plastisol, PVC sol, which is mainly made of PVC powder and additives such as plasticizers through high-speed stirring. In the process of paste making, various fillers, diluents, heat stabilizers, foaming agents and light stabilizers can be added according to the needs of different products.

[0003] PVC paste resin has good chemical stability and certain mechanical strength. It can be used in the production of artificial leather, vinyl toys, soft trademarks, wallpaper, paint coatings, foamed plastics, PVC film materials, etc. When preparing finished products such as PVC film materials, heating and extrusion are common process steps, but in this process, the PVC paste resin often sticks to the roller due to heating. In industrial production, it is currently impossible to predict the roller sticking of PVC paste resin in advance. When the roller sticking phenomenon occurs, it can only be overcome by cooling down.

[0004] After analysis, it was found that the stickiness of PVC paste resin is related to complex factors such as the content and dispersion state of free plasticizers. However, there is a lack of simple and applicable online analysis methods to predict the stickiness of PVC paste resin in advance. Summary of the invention

[0005] In view of the above technical problems, the object of the present invention is to provide a method for predicting the roller sticking property of PVC paste resin. To achieve the above object, the method of the present invention is as follows: A method for predicting PVC paste resin roll adhesion, comprising the steps of: S1: Take a PVC paste resin sample and place it in a test container, which is placed between the rotor and the temperature control platform of the rotational rheometer, set the rotation amplitude, and perform frequency scanning on the PVC paste resin at a constant temperature to obtain a loss modulus-frequency relationship curve and a storage modulus-frequency relationship curve; S2: According to the loss modulus-frequency relationship curve and the storage modulus-frequency relationship curve, a complex viscosity-angular frequency relationship curve is drawn; S3: Predict the roller stickiness of the PVC paste resin sample based on the angular frequency value of the lowest point of the complex viscosity-angular frequency relationship curve.

[0006] According to the research results, when the angular frequency of the lowest point of the complex viscosity-angular frequency relationship curve is ≥100, the PVC paste resin sample will not stick to the roller; when the angular frequency of the lowest point of the complex viscosity-angular frequency relationship curve is <100, the lower the angular frequency, the higher the degree of sticking.

[0007] Preferably, in step S1, the rotation amplitude is 20 rad / s to 30 rad / s.

[0008] Preferably, in step S1, the constant temperature is 150°C to 170°C.

[0009] Preferably, in step S1, the diameter of the rotor is 20 mm to 30 mm.

[0010] Preferably, in step S1, the distance between the rotor and the temperature control platform is 450 μm-550 μm.

[0011] Preferably, in step S1, the volume of the PVC paste resin sample is 1 mL to 5 mL.

[0012] Preferably, in step S3, the angular frequency value of the lowest point of the complex viscosity-angular frequency relationship curve is set at 100 as a judgment threshold.

[0013] Preferably, the PVC paste resin contains PVC resin, filler, plasticizer and viscosity reducer.

[0014] Preferably, the PVC paste resin further contains a flame retardant and / or an anti-ultraviolet agent.

[0015] Preferably, the PVC resin is selected from at least one of SY-Z140, P-440 and SG-3.

[0016] Preferably, the plasticizer is selected from at least one of DINP (diisononyl phthalate), DOP (dioctyl phthalate), and DOA (dioctyl adipate).

[0017] Preferably, the filler is calcium carbonate.

[0018] Beneficial effects of the present invention: (1) The method for predicting the roller sticking property of PVC paste resin of the present invention is suitable for timely online rapid analysis of PVC paste resin, so as to prevent roller sticking before it occurs, avoiding the process complication of adjusting temperature to control roller sticking afterwards.

[0019] (2) The method for predicting the roller adhesion of PVC paste resin of the present invention has no special requirements on the materials used in the formulation of PVC paste resin, and thus has a wide range of applications.

[0020] (3) The method for predicting the roller stickiness of PVC paste resin of the present invention is simple to operate and suitable for promotion.

[0021] (4) According to the method for predicting the roller stickiness of PVC paste resin of the present invention, the formula of PVC paste resin can be adjusted and tested in reverse, thereby realizing the formula optimization of PVC paste resin before the workshop equipment is started, providing a basis for the formula optimization of PVC paste resin and facilitating the process connection of the production workshop. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 The complex viscosity-angular frequency relationship curve of the sample in Example 1 of the present invention; Figure 2 The complex viscosity-angular frequency relationship curve of the sample in Example 2 of the present invention; Figure 3 This is the complex viscosity-angular frequency relationship curve of the sample in Example 3 of the present invention. DETAILED DESCRIPTION

[0023] The present invention will be further described below in conjunction with specific embodiments. It should be understood that the specific embodiments are only used to explain the present invention and are not used to limit the scope of protection of the present invention.

[0024] In the following examples, the rotational rheometer used is the DHR-2 of TA Company of the United States. The software used to draw the complex viscosity-angular frequency relationship curve based on the loss modulus-frequency relationship curve and the storage modulus-frequency relationship curve is TAInstruments TRIOS. The extrusion equipment used is the PVC and PTFE membrane coating immersion test line from Siltes Coating Composite Mechanical Engineering Co., Ltd. of Italy; the sample weight on the machine is 1030±5g, and the machine temperature is 150℃~170℃.

[0025] Example 1 Preparation and testing of PVC paste resin samples (1) 60 parts by weight of PVC resin (SY-Z140 from Tangshan Sanyou Chlor-Alkali Co., Ltd.), 60 parts by weight of filler (activated calcium carbonate KL-10 from Guangxi Hezhou Kelong Powder Co., Ltd.), 60 parts by weight of plasticizer (DINP from Shanghai Hongzhuang Chemical Technology Co., Ltd.), 5 parts by weight of viscosity reducer (D-80 from Shandong Taixi Chemical Co., Ltd.), 2 parts by weight of flame retardant (YS-F2 from Nantong Yasi Flame Retardant Technology Co., Ltd.), and 1 part by weight of anti-ultraviolet agent (UV-328 from Jining Tangyi Chemical Co., Ltd.) were mixed and stirred to obtain PVC paste resin sample A.

[0026] (2) PVC paste resin sample A was adjusted with a plasticizer to obtain PVC paste resin sample B, PVC paste resin sample C and PVC paste resin sample D (the total amount of plasticizer added was 80, 100 and 120 parts by weight, respectively).

[0027] (3) Take 5 mL of PVC paste resin samples A, B, C, and D respectively and place them between the rotor and the temperature control platform of the rotational rheometer. The rotor diameter is 25 mm and the distance between the rotor and the temperature control platform is 500 μm. The rotor of the rotational rheometer is set to a fixed rotation amplitude and a frequency scan is performed at a constant temperature, wherein the rotation amplitude is 20 rad / s and the temperature is 160°C.

[0028] (4) The loss modulus-frequency relationship curve and storage modulus-frequency relationship curve of the PVC paste resin sample were obtained by rotational rheometer testing, and the complex viscosity-angular frequency relationship curve was obtained by calculation and plotting (such as Figure 1 ).

[0029] (5) Analyze the complex viscosity-angular frequency relationship curve and obtain the numerical value of the angular frequency at the lowest point of the curve.

[0030] (6) PVC paste resin samples A, B, C, and D were heated and extruded (150°C to 170°C) to test whether the samples stick to the roller at different temperatures.

[0031] Table 1 shows the actual production status of the PVC paste resin samples of the four formulations and the status of the products produced. When the angular frequency value of the lowest point of the complex viscosity-angular frequency relationship curve is greater than or equal to 100, there is no sticking to the roller within the process temperature range (PVC paste resin samples A and B); when the angular frequency is less than 100, the smaller the value, the more serious the sticking to the roller (PVC paste resin samples C and D).

[0032] Table 1 Angular frequency and machine conditions of different paste resins

[0033] Example 2 Preparation and testing of PVC paste resin samples (1) 60 parts by weight of PVC resin (Shandong Yuquan New Material Technology Co., Ltd., P-440), 60 parts by weight of plasticizer (Jinan Zekuan Chemical Co., Ltd., DOP), 70-110 parts by weight of filler (Jiangxi Guangyuan Group, heavy calcium carbonate CC-600), 3 parts by weight of viscosity reducer (Guangzhou Guangwan New Material Co., Ltd., D-80), 1 part by weight of flame retardant (Changzhou Jili New Material Technology Co., Ltd., antimony trioxide), and 2 parts by weight of anti-ultraviolet agent (Shanghai Kaiyin Chemical Co., Ltd., UV-P) were mixed and stirred to obtain PVC paste resin sample E, PVC paste resin sample F and PVC paste resin sample G (the total amount of filler added was 70, 90, and 110 parts by weight, respectively).

[0034] (2) Take 3 mL of each of PVC paste resin samples E, F, and G and place them between the rotor and the temperature control platform of the rotational rheometer. The rotor diameter is 20 mm and the distance between the rotor and the temperature control platform is 450 μm. The rotor of the rotational rheometer is set to a fixed rotation amplitude and a frequency scan is performed at a constant temperature, wherein the rotation amplitude is 30 rad / s and the temperature is 170°C.

[0035] (3) The loss modulus-frequency relationship curve and storage modulus-frequency relationship curve of the PVC paste resin sample were obtained by rotational rheometer testing, and the complex viscosity-angular frequency relationship curve was obtained by calculation and plotting (such as Figure 2 ).

[0036] (4) Analyze the complex viscosity-angular frequency relationship curve and obtain the numerical value of the angular frequency at the lowest point of the curve.

[0037] (5) PVC paste resin samples E, F, and G were heated and extruded (150°C to 170°C) to test whether the samples stick to the roller at different temperatures.

[0038] Table 2 shows the actual production conditions of the PVC paste resin samples of three formulations and the conditions of the products produced. When the angular frequency value of the lowest point of the complex viscosity-angular frequency relationship curve is greater than or equal to 100, there is no roller sticking phenomenon within the process temperature range; when the angular frequency value is less than 100, the smaller the value, the more serious the roller sticking.

[0039] Table 2 Angular frequency and machine status of different paste resins

[0040] Example 3 Preparation and testing of PVC paste resin samples (1) 60 parts by weight of PVC resin (SG-3, Wuhan Xindongyi Chemical Co., Ltd.), 70 parts by weight of plasticizer (DOA, Shandong Xinghai Chemical Co., Ltd.), 100 parts by weight of filler (heavy calcium carbonate, Haicheng Chengxin Fine Mesh Stone Powder Factory), 6 parts by weight of viscosity reducer (D-80, Shanghai Xinlong Yuteng Chemical Co., Ltd.), 2 parts by weight of flame retardant (K-900, Suzhou Jiayi Chemical Co., Ltd.), and 2 parts by weight of anti-ultraviolet agent (UV-770, Changzhou Youfeng Chemical Co., Ltd.) were mixed and stirred to obtain a PVC paste resin.

[0041] (2) According to the different mesh sizes of the added fillers, the PVC paste resins are divided into PVC paste resin sample H (the added filler is 600 mesh calcium carbonate), PVC paste resin sample I (the added filler is 800 mesh calcium carbonate) and PVC paste resin sample J (the added filler is 1000 mesh calcium carbonate).

[0042] (3) Take 2 mL of each of PVC paste resin samples H, I, and J and place them between the rotor and the temperature control platform of the rotational rheometer. The rotor diameter is 20 mm and the distance between the rotor and the temperature control platform is 450 μm. The rotor of the rotational rheometer is set to a fixed rotation amplitude and a frequency sweep is performed at a constant temperature, wherein the rotation amplitude is 30 rad / s and the temperature is 150°C.

[0043] (4) The loss modulus-frequency relationship curve and storage modulus-frequency relationship curve of the PVC paste resin sample were obtained by rotational rheometer testing, and the complex viscosity-angular frequency relationship curve was obtained by calculation and plotting (such as Figure 3 ).

[0044] (5) Analyze the complex viscosity-angular frequency relationship curve and obtain the numerical value of the angular frequency at the lowest point of the curve.

[0045] (6) PVC paste resin samples H, I, and J were heated and extruded (150°C to 170°C) to test whether the samples stick to the roller at different temperatures.

[0046] Table 3 shows the actual production conditions of the PVC paste resin samples of the three formulations and the conditions of the products produced. When the angular frequency value of the lowest point of the complex viscosity-angular frequency relationship curve is greater than or equal to 100, no roller sticking phenomenon occurs within the process temperature range (PVC paste resin sample J); when the angular frequency is less than 100, the smaller the value, the more serious the roller sticking (PVC paste resin samples H, I).

[0047] Table 3 Angular frequency and machine status of different paste resins

[0048] The method of the present invention has been promoted and tested in actual production, and more than 500 batches of test samples have been tested. The prediction conclusions of the method are consistent with the actual conditions.

[0049] The above embodiments are preferred implementation schemes of the present invention, but do not mean that the implementation scope of the present invention is limited by the above embodiments. Therefore, any other forms, modifications, substitutions, and simplifications produced without departing from the spirit and principles of the present invention are regarded as equivalent replacement methods and are included in the protection scope of the present invention.

Claims

1. A method for predicting the roller adhesion of PVC paste resin, characterized in that: The steps include: S1: Take a PVC paste resin sample and place it in a test container, which is placed between the rotor and the temperature control platform of the rotational rheometer, set the rotation amplitude, and perform frequency scanning on the PVC paste resin at a constant temperature to obtain a loss modulus-frequency relationship curve and a storage modulus-frequency relationship curve; S2: According to the loss modulus-frequency relationship curve and the storage modulus-frequency relationship curve, a complex viscosity-angular frequency relationship curve is drawn; S3: Predict the roller stickiness of the PVC paste resin sample based on the angular frequency value of the lowest point of the complex viscosity-angular frequency relationship curve.

2. A method for predicting the roller adhesion of PVC paste resin according to claim 1, characterized in that: In step S1, the rotation amplitude is 20rad / s-30rad / s.

3. A method for predicting the roller adhesion of PVC paste resin according to claim 1, characterized in that: In step S1, the constant temperature is 150°C to 170°C.

4. A method for predicting the roller adhesion of PVC paste resin according to claim 1, characterized in that: In step S1, the diameter of the rotor is 20 mm to 30 mm.

5. A method for predicting the roller adhesion of PVC paste resin according to claim 1, characterized in that: In step S1, the distance between the rotor and the temperature control platform is 450 μm to 550 μm.

6. A method for predicting the roller adhesion of PVC paste resin according to claim 1, characterized in that: In step S1, the volume of the PVC paste resin sample is 1 mL to 5 mL.

7. A method for predicting the roller adhesion of PVC paste resin according to claim 1, characterized in that: In step S3, the angular frequency value of the lowest point of the complex viscosity-angular frequency relationship curve is set at 100 as a judgment threshold.

8. A method for predicting the roller adhesion of PVC paste resin according to claim 1, characterized in that: The PVC paste resin contains PVC resin, filler, plasticizer and viscosity reducer.

9. A method for predicting the roller adhesion of PVC paste resin according to claim 8, characterized in that: The PVC paste resin further contains a flame retardant and / or an anti-ultraviolet agent.

10. A method for predicting the roller adhesion of PVC paste resin according to claim 8, characterized in that: The PVC resin is selected from at least one of SY-Z140, P-440 and SG-3.

11. A method for predicting the roller adhesion of PVC paste resin according to claim 8, characterized in that: The plasticizer is selected from at least one of DINP, DOP and DOA.

12. The method for predicting the roller adhesion of PVC paste resin according to claim 8, characterized in that: The filler is calcium carbonate.

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