A method for predicting the roll sticking property of PVC paste resin

Abstract

The present 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. In this method, a rotational rheometer is used to perform frequency scanning on the PVC paste resin at a fixed amplitude and a constant temperature to obtain a loss modulus-frequency relationship curve and a storage modulus-frequency relationship curve, and then a complex viscosity-angular frequency relationship curve is plotted. The roll sticking property of the PVC paste resin sample is predicted through the angular frequency value at the lowest point of the complex viscosity-angular frequency relationship curve. This method is suitable for on-line analysis and prediction of the roll sticking property of PVC paste resin, thereby avoiding adjusting the processing temperature after roll sticking occurs, resulting in time-consuming and complicated processes. The invention is simple and reliable, has a wide application range, and is suitable for popularization and application in industrial production.

Description

Technical Field

[0001] The present 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. Background Art

[0002] Polyvinyl chloride (PVC) paste resin, also known as PVC plasticizer paste and PVC sol, is mainly prepared by high-speed stirring of PVC powder and additives such as plasticizers. During the paste preparation process, various fillers, diluents, heat stabilizers, blowing agents, and light stabilizers can be added according to different product requirements.

[0003] PVC paste resin has good chemical stability and certain mechanical strength, and can be used in the production of artificial leather, slush toys, soft trademarks, wallpaper, paint coatings, foamed plastics, PVC films, etc. When preparing finished products such as PVC films, heating and extrusion are common process steps, but the phenomenon of PVC paste resin sticking to the roll often occurs during this process. In industrial production, currently, it is impossible to predict the roll sticking property of PVC paste resin in advance. Only when the roll sticking phenomenon occurs, the subsequent roll sticking is overcome by cooling.

[0004] Through analysis, it is found that the roll sticking of PVC paste resin is related to complex factors such as the content and dispersion state of free plasticizer in it. However, there is a lack of a simple and applicable method for on-line analysis to predict the roll sticking property of PVC paste resin in advance. Summary of the Invention

[0005] Aiming at the above technical problems, the purpose of the present invention is to provide a method for predicting the roll sticking property of PVC paste resin. To achieve the above purpose, the method of the present invention is as follows:

[0006] A method for predicting the roll sticking property of PVC paste resin, comprising the following steps:

[0007] S1: Take a PVC paste resin sample and place it in a test container. The test container is placed between the rotor and the temperature control platform of a rotational rheometer. Set the rotation amplitude and perform a frequency sweep on the PVC paste resin at a constant temperature to obtain a loss modulus - frequency relationship curve and a storage modulus - frequency relationship curve;

[0008] S2: According to the loss modulus - frequency relationship curve and the storage modulus - frequency relationship curve, plot a complex viscosity - angular frequency relationship curve;

[0009] S3: Predict the roll sticking property of the PVC paste resin sample according to the angular frequency value at the lowest point of the complex viscosity - angular frequency relationship curve.

[0010] According to the research results, when the angular frequency at the lowest point of the complex viscosity - angular frequency relationship curve ≥ 100, the PVC paste resin sample does not stick to the roller; when the angular frequency at the lowest point of the complex viscosity - angular frequency relationship curve < 100, the lower the angular frequency, the higher the degree of sticking to the roller.

[0011] Preferably, in step S1, the rotation amplitude is 20 rad / s to 30 rad / s.

[0012] Preferably, in step S1, the constant temperature is 150 °C to 170 °C.

[0013] Preferably, in step S1, the diameter of the rotor is 20 mm to 30 mm.

[0014] Preferably, in step S1, the distance between the rotor and the temperature control platform is 450 μm to 550 μm.

[0015] Preferably, in step S1, the volume of the PVC paste resin sample is 1 mL to 5 mL.

[0016] Preferably, in step S3, the angular frequency value at the lowest point of the complex viscosity - angular frequency relationship curve takes 100 as the judgment boundary value.

[0017] Preferably, the PVC paste resin contains PVC resin, filler, plasticizer, and viscosity reducer.

[0018] Preferably, the PVC paste resin further contains a flame retardant and / or an ultraviolet resistant agent.

[0019] Preferably, the PVC resin is selected from at least one of SY - Z140, P - 440, and SG - 3.

[0020] Preferably, the plasticizer is selected from at least one of DINP (diisononyl phthalate), DOP (dioctyl phthalate), and DOA (dioctyl adipate).

[0021] Preferably, the filler is calcium carbonate.

[0022] Advantages of the present invention:

[0023] (1) The method for predicting the stickiness of PVC paste resin of the present invention is suitable for rapid on - line analysis of PVC paste resin in a timely manner, so as to prevent before stickiness occurs and avoid the problem of the complexity of the process of adjusting the temperature to control stickiness afterwards.

[0024] (2) The method for predicting the stickiness of PVC paste resin of the present invention has no special requirements for the formulation materials of PVC paste resin, so it has a wide application range.

[0025] (3) The method for predicting the roll sticking property of PVC paste resin according to the present invention is simple to operate and suitable for popularization.

[0026] (4) According to the method for predicting the roll sticking property of PVC paste resin of the present invention, the formulation of PVC paste resin can be adjusted and tested in reverse, so as to optimize the formulation of PVC paste resin before the start-up of workshop equipment, provide a basis for the formulation optimization of PVC paste resin, and facilitate the process connection of the production workshop. Description of the Drawings

[0027] Figure 1 It is the curve of complex viscosity - angular frequency relationship of the sample in Example 1 of the present invention;

[0028] Figure 2 It is the curve of complex viscosity - angular frequency relationship of the sample in Example 2 of the present invention;

[0029] Figure 3 It is the curve of complex viscosity - angular frequency relationship of the sample in Example 3 of the present invention. Detailed Embodiments

[0030] The present invention will be further described below with reference to 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 protection scope of the present invention.

[0031] In the following embodiments, the rotational rheometer used is DHR-2 of TA Instruments, USA. According to the loss modulus - frequency relationship curve and storage modulus - frequency relationship curve, the software used to plot the complex viscosity - angular frequency relationship curve is TAInstruments TRIOS. The extrusion equipment used is the PVC and PTFE film coating impregnation test line from Silter Coating Composite Machinery Engineering Co., Ltd., Italy; the sample weight on the machine is 1030 ± 5 g, and the temperature on the machine is 150°C to 170°C.

[0032] Example 1 Preparation and Testing of PVC Paste Resin Sample

[0033] (1) 60 parts by weight of PVC resin (Tangshan Sanyou Chlor-Alkali Co., Ltd., SY-Z140), 60 parts by weight of filler (Guangxi Hezhou Kelong Powder Co., Ltd., activated calcium carbonate KL-10), 60 parts by weight of plasticizer (Shanghai Hongzhuang Chemical Technology Co., Ltd., DINP), 5 parts by weight of viscosity reducer (Shandong Taixi Chemical Co., Ltd., D-80), 2 parts by weight of flame retardant (Nantong Yasi Flame Retardant Technology Co., Ltd., YS-F2), and 1 part by weight of ultraviolet absorber (Jining Tangyi Chemical Co., Ltd., UV-328) are mixed and stirred to obtain PVC paste resin sample A.

[0034] (2) The plasticizer was used to adjust PVC paste resin sample A to obtain PVC paste resin samples B, C, and D (the total addition amounts of the plasticizer were 80, 100, and 120 parts by weight, respectively).

[0035] (3) 5 mL of each of PVC paste resin samples A, B, C, and D was taken and placed between the rotor and the temperature-controlled platform of a rotational rheometer. The rotor diameter was 25 mm, and the distance between the rotor and the temperature-controlled platform was 500 μm. The rotor of the rotational rheometer was set to a fixed rotation amplitude, and frequency scanning was performed at a constant temperature, where the rotation amplitude was 20 rad / s and the temperature was 160 °C.

[0036] (4) The loss modulus - frequency relationship curve and the storage modulus - frequency relationship curve of the PVC paste resin samples were obtained through testing with the rotational rheometer, and the complex viscosity - angular frequency relationship curve was obtained by calculation and plotting (as Figure 1 ).

[0037] (5) The complex viscosity - angular frequency relationship curve was analyzed to obtain the value of the angular frequency at the lowest point of the curve.

[0038] (6) PVC paste resin samples A, B, C, and D were heated and extruded on a machine (150 °C - 170 °C), and whether the samples stuck to the roll at different temperatures was tested.

[0039] Table 1 shows the on-machine conditions of the PVC paste resin samples of the four formulations during actual production and the conditions of the products produced. When the value of the angular frequency at the lowest point of the complex viscosity - angular frequency relationship curve is greater than or equal to 100, no roll sticking phenomenon occurs 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 roll sticking (PVC paste resin samples C and D).

[0040] Table 1 Angular Frequencies and On-Machine Conditions of Different Paste Resins

[0041]

[0042] Example 2 Preparation and Testing of PVC Paste Resin Samples

[0043] (1) Mix 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 UV absorber (Shanghai Kayin Chemical Co., Ltd., UV-P) to obtain PVC paste resin samples E, F, and G (with total filler addition amounts of 70, 90, and 110 parts by weight respectively).

[0044] (2) Take 3 mL each of PVC paste resin samples E, F, and G and place them between the rotor and the temperature control platform of a rotational rheometer. The rotor diameter is 20 mm, and the distance between the rotor and the temperature control platform is 450 μm. Set the rotor of the rotational rheometer to a fixed rotation amplitude and perform frequency scanning at a constant temperature, where the rotation amplitude is 30 rad / s and the temperature is 170 °C.

[0045] (3) Obtain the loss modulus - frequency relationship curve and storage modulus - frequency relationship curve of the PVC paste resin samples through testing with a rotational rheometer, and obtain the complex viscosity - angular frequency relationship curve by calculation and plotting (as Figure 2 ).

[0046] (4) Analyze the complex viscosity - angular frequency relationship curve to obtain the value of the angular frequency at the lowest point of the curve.

[0047] (5) Heat and extrude PVC paste resin samples E, F, and G on a machine (150 °C - 170 °C) to test whether the samples stick to the roll at different temperatures.

[0048] Table 2 shows the on-machine conditions of PVC paste resin samples with three formulations during actual production and the conditions of the products produced. When the value of the angular frequency at the lowest point of the complex viscosity - angular frequency relationship curve is greater than or equal to 100, there is no roll sticking phenomenon within the process temperature range; when the angular frequency value is less than 100, the smaller the value, the more serious the roll sticking.

[0049] Table 2 Angular Frequencies and On-Machine Conditions of Different Paste Resins

[0050]

[0051] Preparation and Testing of PVC Paste Resin Samples in Example 3

[0052] (1) Mix 60 parts by weight of PVC resin (Wuhan Xindongyi Chemical Co., Ltd., SG-3), 70 parts by weight of plasticizer (Shandong Xinghai Chemical Co., Ltd., DOA), 100 parts by weight of filler (Haicheng Chengxin Micro Mesh Stone Powder Factory, heavy calcium carbonate), 6 parts by weight of viscosity reducer (Shanghai Xinlongyuteng Chemical Co., Ltd., D-80), 2 parts by weight of flame retardant (Suzhou Jiayi Chemical Co., Ltd., K-900), and 2 parts by weight of UV absorber (Changzhou Youfeng Chemical Co., Ltd., UV-770) and stir to obtain PVC paste resin.

[0053] (2) According to the different mesh numbers of the added filler, divide the PVC paste resin 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).

[0054] (3) Take 2 mL of each of PVC paste resin samples H, I, and J and place them between the rotor and the temperature-controlled platform of a rotational rheometer. The rotor diameter is 20 mm, and the distance between the rotor and the temperature-controlled platform is 450 μm. Set the rotor of the rotational rheometer to a fixed rotation amplitude and perform a frequency sweep at a constant temperature, where the rotation amplitude is 30 rad / s and the temperature is 150 °C.

[0055] (4) Obtain the loss modulus-frequency relationship curve and storage modulus-frequency relationship curve of the PVC paste resin sample through testing with a rotational rheometer, and obtain the complex viscosity-angular frequency relationship curve by calculation and plotting (as Figure 3 ).

[0056] (5) Analyze the complex viscosity-angular frequency relationship curve to obtain the value of the angular frequency at the lowest point of the curve.

[0057] (6) Heat and extrude PVC paste resin samples H, I, and J on a machine (150 °C - 170 °C) and test whether the samples stick to the roller at different temperatures.

[0058] Table 3 shows the on-machine conditions of PVC paste resin samples of three formulations during actual production and the conditions of the products produced. When the value of the angular frequency at the lowest point of the complex viscosity-angular frequency relationship curve is greater than or equal to 100, there is no phenomenon of sticking to the roller 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 sticking to the roller (PVC paste resin samples H, I).

[0059] Table 3 Angular Frequencies and On-Machine Conditions of Different Paste Resins

[0060]

[0061] The method of the present invention has been promoted and tested in actual production. The number of test samples has exceeded 500 batches, and the prediction conclusions of this method are all consistent with the actual situation on the machine.

[0062] The above embodiments are preferred implementation schemes of the present invention, and do not represent that the implementation scope of the present invention is limited by the above embodiments. Therefore, any other forms, modifications, substitutions, and simplifications generated without departing from the spirit and principle of the present invention are regarded as equivalent replacement methods and are all 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: predicting the roller stickiness of the PVC paste resin sample according to the angular frequency value of the lowest point of the complex viscosity-angular frequency relationship curve; The PVC paste resin contains PVC resin, filler, plasticizer, and viscosity reducer; the plasticizer is selected from at least one of DINP, DOP, and DOA; the filler is calcium carbonate; the PVC resin is selected from at least one of SY-Z140, P-440, and SG-3; the viscosity reducer is D-80; and the extrusion temperature of the PVC paste resin is 150° C. to 170° C.

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 further contains a flame retardant and / or an anti-ultraviolet agent.

Images