Formula and preparation method of high-brightness polyester chip

Abstract

The invention relates to a high-brightness polyester chip formula, which comprises the following substance components: terephthalic acid, ethylene glycol, an ethylene glycol antimony solution and a phosphoric acid solution. Wherein the molar ratio of the terephthalic acid to the ethylene glycol is (1: 1.10)-(1: 1.20); the adding amount of the ethylene glycol antimony solution is 0.040 wt%-0.050 wt% of the adding amount of the terephthalic acid; by adding phosphoric acid, thermal degradation of polyester melt at high temperature can be effectively reduced, so that darkening and brightness reduction caused by thermal degradation are avoided, the polyester chip produced by the method has higher brightness and more uniform color, and the use of a fluorescent whitening agent is avoided, so that the environmental protection performance of the product is remarkably improved, and the production cost is reduced. The polyester chip prepared by the method can meet the strict requirements of high-end application fields on product appearances, such as high-quality textiles and films, thermal degradation is reduced, the integrity of polyester molecular chains can be maintained, so that the molecular weight of the polyester chip is improved, and when the polyester chip with high molecular weight is processed into fibers or films, a tighter molecular chain structure can be formed.

Description

Technical Field

[0001] The invention relates to the technical field of polyester chip processing, and in particular to a high-brightness polyester chip formula and a preparation method. Background Art

[0002] When processed into fibers, films and other products, high-brightness polyester chips can exhibit higher gloss and more uniform color, making the products more visually attractive and meeting the stringent appearance requirements of high-end applications such as high-quality textiles, packaging materials, and decorative materials. As consumers' requirements for product quality and appearance continue to increase, high-brightness polyester chips can better meet the needs of high-end markets such as high-end textiles, automotive interiors, and electronic films, helping companies to expand into high-end markets and increase their market share. At present, there are two main methods to improve the brightness of polyester chips: one is to add additives such as fluorescent brighteners during the production process of polyester chips, and the other is to use special polymerization processes and formulas. However, the use of fluorescent brighteners will affect the environmental performance of polyester chips, and special polymerization processes and formulas will increase production costs. In order to solve the above problems, the present invention proposes a high-brightness polyester chip formula and preparation method. Summary of the Invention

[0003] (1) Technical problems to be solved The purpose of the present invention is to reduce production costs while ensuring the environmental performance of polyester chips. To this end, the present invention provides a high-brightness polyester chip formula and preparation method.

[0004] (2) Technical solution In order to achieve the purpose of the present invention, the technical solution adopted by the present invention is: A high-brightness polyester chip formula comprises the following material components: terephthalic acid, ethylene glycol, ethylene glycol antimony solution and phosphoric acid solution; Wherein, the molar ratio of terephthalic acid to ethylene glycol is 1:1.10 to 1:1.20, the molar mass of terephthalic acid is about 166.13 g / mol, the mass of terephthalic acid is divided by its molar mass to obtain the molar number of terephthalic acid, the molar ratio of terephthalic acid to ethylene glycol is known, the molar number of terephthalic acid is multiplied by the molar ratio to obtain the molar number of ethylene glycol, and the molar mass of ethylene glycol is about 62.07 g / mol, the molar number of ethylene glycol is multiplied by its molar mass , which is the mass of ethylene glycol; the amount of ethylene glycol antimony solution added is 0.040wt% to 0.050wt% of the amount of terephthalic acid added, and the amount of ethylene glycol antimony solution added should be controlled between 0.040% and 0.050% of the mass of terephthalic acid; the amount of phosphoric acid solution added is 0.0005wt% to 0.0007wt% of the amount of terephthalic acid added, and the amount of phosphoric acid solution added should be controlled between 0.050% and 0.070% of the mass of terephthalic acid.

[0005] Furthermore, the solute ratio of the phosphoric acid solution is 4.5% to 5.5%, and the mass of phosphoric acid accounts for a proportion of the total mass of the solution between 4.5% and 5.5%.

[0006] Furthermore, the solute ratio of the ethylene glycol antimony solution is 2.0% to 2.5%, and the mass of the ethylene glycol antimony accounts for 2.0% to 2.5% of the total mass of the solution.

[0007] A method for preparing the above-mentioned high-brightness polyester chip formula comprises the following steps: S1: After terephthalic acid, ethylene glycol, ethylene glycol antimony solution and phosphoric acid solution are uniformly mixed, the mixture is pressurized and sent to the esterification reactor by a screw pump to carry out esterification reaction; S2: After the esterification reaction is completed, the polycondensation reaction in the low vacuum stage begins under negative pressure conditions. In this stage, the pressure is steadily pumped from normal pressure to an absolute pressure below 500 Pa; S3: After the polycondensation reaction in the low vacuum stage is completed, continue to evacuate the vacuum to carry out the polycondensation reaction in the high vacuum stage, so that the reaction pressure drops to below 100 Pa absolute pressure; S4: After the polycondensation reaction in the high vacuum stage is completed, the reactants are pressurized and sent to the precision filter for filtration through a gear pump; S5: The filtered reactants are sent to a pelletizer for cooling and pelletizing to obtain high-brightness polyester chips.

[0008] Furthermore, the pressure of the esterification reaction in step S1 is normal pressure to 70 kPa, and the temperature of the esterification reaction is 250 to 260°C.

[0009] Furthermore, the esterification reaction in step S1 is terminated when the amount of water distilled out reaches 90% of the theoretical value.

[0010] Furthermore, the reaction temperature of the polycondensation reaction in the initial low vacuum stage in step S2 is 250-260° C., and the reaction time is 30-50 min.

[0011] Furthermore, the reaction temperature of the polycondensation reaction in the high vacuum stage in step S3 is 270-282° C., and the reaction time is 50-90 min.

[0012] Furthermore, the phosphoric acid solution in step S1 is prepared as follows: Add ethylene glycol to a reactor at 20-30°C, start the stirrer in the reactor, add phosphoric acid with a mass ratio of 4.5% to 5.5% of ethylene glycol, and continue stirring for 10 to 20 minutes to obtain a phosphoric acid solution.

[0013] Furthermore, the preparation method of the ethylene glycol antimony solution in step S1 is: Add ethylene glycol to the reactor at 20-30°C, start the stirrer in the reactor and introduce steam into the coil of the reactor. When the reaction temperature reaches 98°C, add ethylene glycol antimony with a mass ratio of 2.0% to 2.5% of ethylene glycol, and continue stirring for 10 to 20 minutes to obtain ethylene glycol antimony solution.

[0014] (3) Beneficial effects: A. The addition of phosphoric acid in the present invention can effectively reduce thermal degradation of polyester melt at high temperatures, thereby avoiding color darkening and brightness reduction caused by thermal degradation. The polyester chips produced in this way have higher brightness and more uniform color, avoiding the use of fluorescent brighteners, thereby significantly improving the environmental performance of the product and meeting the strict appearance requirements of high-end applications such as high-quality textiles and films. B. The present invention reduces thermal degradation and helps maintain the integrity of the polyester molecular chain, thereby increasing the molecular weight of the polyester chips. When processed into fibers or films, high-molecular-weight polyester chips can form a tighter molecular chain structure, thereby improving the tensile strength and corrosion resistance of the material. This makes products made from high-brightness polyester chips (such as fibers, films, etc.) more durable during use and less likely to break, discolor, or deform. DETAILED DESCRIPTION

[0015] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0016] The present invention will be further described below in conjunction with the embodiments: Example 1: A high-brightness polyester chip formulation comprises the following material components: 1000 g of terephthalic acid, 1110 g of ethylene glycol, 4.5 g of ethylene glycol antimony solution, and 0.5 g of phosphoric acid solution.

[0017] Furthermore, the phosphoric acid solution is prepared as follows: At 20° C., 1110 g of ethylene glycol was added to the reactor, the stirrer was started, 50.5 g of phosphoric acid was added, and the mixture was stirred for 15 minutes to obtain a phosphoric acid solution.

[0018] Furthermore, the preparation method of the ethylene glycol antimony solution is: At 20°C, 1110 g of ethylene glycol was added to the reactor, the stirrer was started and steam was introduced into the coil. When the reaction temperature reached 98°C, 22.2 g of ethylene glycol antimony was added and stirred for 15 minutes to obtain an ethylene glycol antimony solution.

[0019] A method for preparing the above-mentioned high-brightness polyester chip formula comprises the following steps: S1: 1000g of terephthalic acid, 1110g of ethylene glycol, 4.5g of ethylene glycol antimony solution and 0.5g of phosphoric acid solution were mixed evenly, pressurized to 50kPa by a screw pump, and sent to an esterification reactor for esterification reaction at 255℃ until the water distillate reached 90% of the theoretical value; S2: After the esterification reaction is completed, the polycondensation reaction in the low vacuum stage is started under negative pressure conditions, and the reaction pressure is steadily pumped down to below 300 Pa absolute pressure, the reaction temperature is 255°C, and the reaction time is 40 minutes; S3: After the low vacuum stage, the vacuum is continued to be pumped down to an absolute pressure below 80 Pa, and the polycondensation reaction is carried out in the high vacuum stage. The reaction temperature is 275°C and the reaction time is 70 minutes. S4: After the high vacuum stage, the reactants are pressurized and sent to the precision filter for filtration through the gear pump; S5: The filtered reactants are sent to a pelletizer for cooling and pelletizing to obtain high-brightness polyester chips.

[0020] Example 2: A high-brightness polyester chip formulation comprises the following material components: 1000 g of terephthalic acid, 1150 g of ethylene glycol, 5.0 g of ethylene glycol antimony solution, and 0.6 g of phosphoric acid solution.

[0021] Furthermore, the phosphoric acid solution is prepared as follows: At 25° C., 1150 g of ethylene glycol was added to the reactor, the stirrer was started, 57.5 g of phosphoric acid was added, and the mixture was stirred for 12 minutes to obtain a phosphoric acid solution.

[0022] Furthermore, the preparation method of the ethylene glycol antimony solution is: At 25°C, 1150g of ethylene glycol was added to the reactor, the stirrer was started and steam was introduced into the coil. When the reaction temperature reached 98°C, 28.75g of ethylene glycol antimony was added and stirred for 12 minutes to obtain an ethylene glycol antimony solution.

[0023] A method for preparing the above-mentioned high-brightness polyester chip formula comprises the following steps: S1: 1000 g of terephthalic acid, 1150 g of ethylene glycol, 5.0 g of ethylene glycol antimony solution and 0.6 g of phosphoric acid solution were mixed evenly, pressurized to 60 kPa by a screw pump, and sent to an esterification reactor for esterification reaction at 250 ° C until the water distillate reached 90% of the theoretical value; S2: After the esterification reaction is completed, the polycondensation reaction in the low vacuum stage is started under negative pressure conditions, and the reaction pressure is steadily pumped down to below 400 Pa absolute pressure, the reaction temperature is 260 ° C, and the reaction time is 30 minutes; S3: After the low vacuum stage, the vacuum is continued to be pumped to an absolute pressure below 90 Pa, and the polycondensation reaction is carried out in the high vacuum stage. The reaction temperature is 282°C and the reaction time is 50 minutes; S4: After the high vacuum stage, the reactants are pressurized and sent to the precision filter for filtration through the gear pump; S5: The filtered reactants are sent to a pelletizer for cooling and pelletizing to obtain high-brightness polyester chips.

[0024] Example 3: A high-brightness polyester chip formulation comprises the following material components: 1000 g of terephthalic acid, 1200 g of ethylene glycol, 4.8 g of ethylene glycol antimony solution, and 0.7 g of phosphoric acid solution.

[0025] Furthermore, the phosphoric acid solution is prepared as follows: At 30° C., 1200 g of ethylene glycol was added to the reactor, the stirrer was started, 60.0 g of phosphoric acid was added, and the mixture was stirred for 10 minutes to obtain a phosphoric acid solution.

[0026] Furthermore, the preparation method of the ethylene glycol antimony solution is: At 30°C, 1200g of ethylene glycol was added to the reactor, the stirrer was started and steam was introduced into the coil. When the reaction temperature reached 98°C, 26.4g of ethylene glycol antimony was added and stirred for 10 minutes to obtain an ethylene glycol antimony solution.

[0027] A method for preparing the above-mentioned high-brightness polyester chip formula comprises the following steps: S1: 1000 g of terephthalic acid, 1200 g of ethylene glycol, 4.8 g of ethylene glycol antimony solution and 0.7 g of phosphoric acid solution were mixed evenly, pressurized to 70 kPa by a screw pump, and sent to an esterification reactor for esterification reaction at 260 ° C until the water distillate reached 90% of the theoretical value; S2: After the esterification reaction is completed, the polycondensation reaction in the low vacuum stage is started under negative pressure conditions, and the reaction pressure is steadily pumped down to below 500 Pa absolute pressure, the reaction temperature is 250°C, and the reaction time is 50 minutes; S3: After the low vacuum stage, continue to evacuate to an absolute pressure below 100 Pa and perform a high vacuum stage polycondensation reaction at a reaction temperature of 270°C and a reaction time of 90 minutes; S4: After the high vacuum stage, the reactants are pressurized and sent to the precision filter for filtration through the gear pump; S5: The filtered reactants are sent to a pelletizer for cooling and pelletizing to obtain high-brightness polyester chips.

[0028] Example 4: A high-brightness polyester chip formulation comprises the following material components: 1000 g of terephthalic acid, 1130 g of ethylene glycol, and 4.6 g of ethylene glycol antimony solution.

[0029] Furthermore, the preparation method of the ethylene glycol antimony solution is: At 22°C, 1130 g of ethylene glycol was added to the reactor, the stirrer was started, and steam was introduced into the coil. When the reaction temperature reached 98°C, 26.0 g of ethylene glycol antimony was added and stirred for 18 minutes to obtain an ethylene glycol antimony solution.

[0030] A method for preparing the above-mentioned high-brightness polyester chip formula comprises the following steps: S1: 1000g of terephthalic acid, 1130g of ethylene glycol, and 4.6g of ethylene glycol antimony solution were mixed evenly, pressurized to 55kPa by a screw pump, and sent to an esterification reactor for esterification reaction at 258°C until the water distillate reached 90% of the theoretical value; S2: After the esterification reaction is completed, the polycondensation reaction in the low vacuum stage is started under negative pressure conditions, and the reaction pressure is steadily pumped down to below 500 Pa absolute pressure, the reaction temperature is 250°C, and the reaction time is 50 minutes; S3: After the low vacuum stage, continue to evacuate to an absolute pressure below 100 Pa and perform a high vacuum stage polycondensation reaction at a reaction temperature of 270°C and a reaction time of 90 minutes; S4: After the high vacuum stage, the reactants are pressurized and sent to the precision filter for filtration through the gear pump; S5: The filtered reactants are sent to a pelletizer for cooling and pelletizing to obtain high-brightness polyester chips.

[0031] The polyester chips obtained in Examples 1, 2, 3 and 4 were subjected to appearance and color testing in the following manner, including the following steps: The polyester chips prepared in the above-mentioned Examples 1, 2, 3 and 4 were photographed and the photographs were retained; Put all the polyester chips into the salt spray test chamber. The salt spray test chamber uses a 5% sodium chloride saline solution with a pH value adjusted to a neutral range (6-7) as the spray solution. The test temperature is 35°C, the air inlet pressure is controlled at 0.3mPa, and the spray pressure is controlled at 0.07-0.17mPa. Take random inspection photos at 2 hours, 8 hours, and 48 hours in the salt spray test chamber, and compare the color of the inspection photos with the original photos. The experimental results are as follows: From the experimental results, we can see that: Examples 1, 2, and 3 are superior to Example 4 in terms of initial brightness, color uniformity, and stability under different environmental conditions, which does not include the addition of phosphoric acid.

[0032] The polyester chips obtained in Examples 1, 2, 3 and 4 were subjected to a tensile test in the following manner, including the following steps: Take the same weight of polyester chips from Example 1, Example 2, Example 3 and the control example, and process the polyester chips into standard tensile test samples to ensure that the size and shape of the samples are consistent; A universal material testing machine was used to perform a tensile test. The test speed was set to 10 mm / min, the test temperature was 25°C, and the humidity was 50%. Each sample was subjected to a tensile test and the elongation at break was recorded. Five samples were tested for each formula, and the average value was taken as the final result. The experimental results are as follows: From the experimental results, we can see that: The elongation at break of Example 1, Example 2, and Example 3 are all superior to that of Example 4 in which phosphoric acid is not added.

[0033] The embodiments disclosed in the present invention are preferred embodiments, but are not limited to them. Ordinary technicians in this field can easily understand the spirit of the present invention based on the above embodiments and make different extensions and changes. As long as they do not deviate from the spirit of the present invention, they are all within the scope of protection of the present invention.

Claims

1. A high brightness polyester chip formula, characterized in that: The invention comprises the following material components: terephthalic acid, ethylene glycol, ethylene glycol antimony solution and phosphoric acid solution; The molar ratio of terephthalic acid to ethylene glycol is 1:1.10 to 1:1.20; the amount of ethylene glycol antimony solution added is 0.040wt% to 0.050wt% of the amount of terephthalic acid added; and the amount of phosphoric acid solution added is 0.0005wt% to 0.0007wt% of the amount of terephthalic acid added.

2. A high brightness polyester chip formula according to claim 1, characterized in that: The solute ratio of the phosphoric acid solution is 4.5% to 5.5%.

3. A high brightness polyester chip formula according to claim 1, characterized in that: The solute ratio of the ethylene glycol antimony solution is 2.0% to 2.5%.

4. A method for preparing the high-brightness polyester chip formula according to claims 1-3, characterized in that: The following steps are involved: S1: After terephthalic acid, ethylene glycol, ethylene glycol antimony solution and phosphoric acid solution are uniformly mixed, the mixture is pressurized and sent to the esterification reactor by a screw pump to carry out esterification reaction; S2: After the esterification reaction is completed, the polycondensation reaction in the low vacuum stage begins under negative pressure conditions. In this stage, the pressure is steadily pumped from normal pressure to an absolute pressure below 500 Pa; S3: After the polycondensation reaction in the low vacuum stage is completed, continue to evacuate the vacuum to carry out the polycondensation reaction in the high vacuum stage, so that the reaction pressure drops to below 100 Pa absolute pressure; S4: After the polycondensation reaction in the high vacuum stage is completed, the reactants are pressurized and sent to the precision filter for filtration through a gear pump; S5: The filtered reactants are sent to a pelletizer for cooling and pelletizing to obtain high-brightness polyester chips.

5. The method for preparing a high-brightness polyester chip formula according to claim 4, wherein: The pressure of the esterification reaction in step S1 is between normal pressure and 70 kPa, and the temperature of the esterification reaction is between 250° C. and 260° C.

6. The method for preparing a high-brightness polyester chip formula according to claim 5, wherein: The esterification reaction in step S1 is terminated when the amount of water distilled out reaches 90% of the theoretical value.

7. The method for preparing a high-brightness polyester chip formulation according to claim 4, wherein: The reaction temperature of the polycondensation reaction in the initial low vacuum stage in step S2 is 250-260° C., and the reaction time is 30-50 min.

8. The method for preparing a high-brightness polyester chip formulation according to claim 4, wherein: The reaction temperature of the polycondensation reaction in the high vacuum stage in step S3 is 270-282° C., and the reaction time is 50-90 min.

9. The method for preparing a high-brightness polyester chip formulation according to claim 4, wherein: The method for preparing the phosphoric acid solution in step S1 is: Add ethylene glycol to a reactor at 20-30°C, start the stirrer in the reactor, add phosphoric acid with a mass ratio of 4.5% to 5.5% of ethylene glycol, and continue stirring for 10 to 20 minutes to obtain a phosphoric acid solution.

10. The method for preparing a high-brightness polyester chip formulation according to claim 4, wherein: The preparation method of the ethylene glycol antimony solution in step S1 is: Add ethylene glycol to the reactor at 20-30°C, start the stirrer in the reactor and introduce steam into the coil of the reactor. When the reaction temperature reaches 98°C, add ethylene glycol antimony with a mass ratio of 2.0% to 2.5% of ethylene glycol, and continue stirring for 10 to 20 minutes to obtain ethylene glycol antimony solution.

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