CN102653591A - Process for producing caprolactam and nylon 66 salt copolymer slice - Google Patents
Process for producing caprolactam and nylon 66 salt copolymer slice Download PDFInfo
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- CN102653591A CN102653591A CN2012101676116A CN201210167611A CN102653591A CN 102653591 A CN102653591 A CN 102653591A CN 2012101676116 A CN2012101676116 A CN 2012101676116A CN 201210167611 A CN201210167611 A CN 201210167611A CN 102653591 A CN102653591 A CN 102653591A
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Abstract
The invention relates to a process for producing a caprolactam and nylon 66 salt copolymer slice. The process comprises the following steps of: 1) preparing raw materials, namely respectively preparing caprolactam melt, a nylon 66 salt aqueous solution and an additive; 2) mixing the raw materials prepared in the step 1) in a mixer; 3) reacting the raw materials mixed in the step 2) in a pre-polymerization tower; 4) reacting the materials treated in the step 3) in a post-polymerization tower for reaction; 5) slicing the materials prepared in the step 4); 6) extracting the slices prepared in the step 5); 7) drying the extracted slices in the step 6); and 8) cooling the slices dried in the step 7), thus obtaining the caprolactam and nylon 66 salt copolymer slice finished product. According to the technical scheme, the caprolactam and nylon 66 salt copolymer slice has the characteristics of outstanding tensile strength, anti-impact strength and anti-puncturing strength, high gas isolation performance, high heat resistance, high mist degree, high glossiness, low temperature performance, flexibility, high transparency, high printablility and the like.
Description
Technical field
The present invention relates to the production technique of a kind of caprolactam and nylon salt multipolymer section.
Background technology
Summary of the invention
Deficiency to the prior art existence; The object of the present invention is to provide a kind of in maintenance nylon 6 its outstanding tensile strength, resistance to impact shock and the anti-intensity that pierces through; Good barrier properties for gases; Outside good thermotolerance, mist degree and glossiness and the good characteristics such as impressionability, have good low-temperature performance, flexibility simultaneously, to prevent that food product pack is in refrigerating process; The packing film hardening, be prone to broken, and the caprolactam with high-clarity more and the nylon salt multipolymer production technique of cutting into slices.
For realizing above-mentioned purpose; 1), the preparation of raw material the invention provides following technical scheme: the production technique of a kind of caprolactam and nylon salt multipolymer section may further comprise the steps:: the aqueous solution and the additive that prepare caprolactam melt, nylon salt respectively; 2) raw material that, step 1) is made is squeezed into mixing tank and is mixed; 3), will be through step 2) the blended material gets into the pre-polymerization tower; Caprolactam quickens open loop and carries out addition and part polycondensation respectively under the effect of water and nylon salt; Obtain the melt of low-molecular-weight caprolactam and nylon salt multipolymer, and in the pre-polymerization tower, slough excessive moisture; 4) the low-molecular-weight caprolactam that, step 3) is made and the melt of nylon salt multipolymer are after film forming device is sloughed residual water-content; Enter into the post polymerization tower; Slough the low-molecular-weight caprolactam of moisture and the melt of nylon salt multipolymer and in the post polymerization tower, carry out copolycondensation and balance, molecular weight is further brought up to the caprolactam of formation desired molecule amount and the melt of nylon salt multipolymer; 5) caprolactam that, step 4) is made and the melt of nylon salt multipolymer carry out pelletizing through dicing machine and obtain caprolactam and cut into slices with the nylon salt multipolymer; 6) caprolactam and the section of nylon salt multipolymer that, step 5) are made extract; 7), will carry out drying through caprolactam after the step 6) extraction and nylon salt multipolymer section entering drying tower; 8), will get into the cooling feed bin through the section of the dried caprolactam of step 7) and nylon salt multipolymer cools off and obtains caprolactam and the nylon salt multipolymer finished product of cutting into slices.
Through adopting technique scheme, caprolactam that makes and the section of nylon salt multipolymer are keeping nylon 6 its outstanding tensile strength, resistance to impact shock and the anti-intensity that pierces through; Good barrier properties for gases outside good thermotolerance, mist degree and glossiness and the good characteristics such as impressionability, has improved low-temperature performance simultaneously; Improved flexibility; Prevent food product pack in refrigerating process, packing film hardening, easy to be broken, and have higher transparency.
The present invention further is set to: the top in the pre-polymerization tower of said step 3) is provided with tubulation; The arranged outside of pre-polymerization tower has insulation jacket; Each is heated the tubulation of said pre-polymerization tower and insulation jacket by one tunnel gas phase heating agent; Pressure in the pre-polymerization tower between 1.5-2.5bar, in the pre-polymerization tower temperature between 245-275 ℃, through step 2) the blended material got in the pre-polymerization tower reservation 4 hours.
Through adopting technique scheme; Caprolactam is under the effect of water and nylon salt; Open loop, addition and part polycondensation can be carried out smoothly, and the low-molecular-weight caprolactam in exit and the melt viscosity of nylon salt multipolymer are controlled at relative viscosity RV2.0-2.1 (96% vitriol oil).
The present invention further is set to: said step 4) also comprises: slough the post polymerization tower internal reaction of melt between 260-265 ℃ 2-3 hour of low-molecular-weight caprolactam and the nylon salt multipolymer of moisture, make molecular weight further improve; Be provided with tubulation in the post polymerization tower; The tubulation of post polymerization tower cools off through the circulation heating agent and removes reaction heat then; Make the insulation balance that material carried out 6-7 hour between 245-255 ℃; Make the molecular chain more even distribution through molecular chain exchange, and reach the caprolactam of desired molecule amount and the melt of nylon salt multipolymer.
Through adopting technique scheme; The melt of low-molecular-weight caprolactam and nylon salt multipolymer can carry out copolycondensation and balance smoothly, and the melt viscosity of caprolactam and nylon salt multipolymer is controlled at relative viscosity RV2.6-2.8 (96% vitriol oil).
The present invention further is set to: said step 1) also comprises: with solid-state caprolactam through kibbler get into the melting still and through the circulation transferpump get into behind the interchanger again through steam heating and with new solid material mixed melting, squeeze into a middle vessel that presss from both sides hot water thermal insulating with pump after filtering through strainer is smart then; Preparing tank at jacketed and whisking appliance adds the hot de-salted water of deoxidation through under meter earlier; Be mixed with 66 salt brine solutions through being metered into solid-state nylon salt through stirring then with water; The preparation temperature is controlled between 75-100 ℃; The concentration of the aqueous solution is controlled at below 60%, and squeezes into the middle vessel of band hot water thermal insulating.
Through adopting technique scheme, make the subsequent production of caprolactam and nylon salt multipolymer section to carry out smoothly.
The present invention further is set to: raw material peace quality is 70-94.9% than caprolactam ratio said step 2), and 66 salt ratios are 30-5%, and additive is 0.05-0.2%.
Through adopting technique scheme, make the subsequent production of caprolactam and nylon salt multipolymer section to carry out smoothly.
The present invention further is set to: said step 6) also comprises: caprolactam that step 5) is made and the section of nylon salt multipolymer divide dried up through drying machine and through being fed into extraction tower behind the vibrosieve divorce particle; In the extraction tower is normal pressure; Be evenly distributed with a lot of cowling panels in the tower so as section from top to bottom, the de-ionized process water of heat is plunger flow from top to bottom, temperature is controlled between 98-110 ℃ in the extraction tower.
Through adopting technique scheme; Make caprolactam monomer and oligopolymer in the section of caprolactam and nylon salt multipolymer carry out the water hot extraction; Low molecule content in caprolactam and the section of nylon salt multipolymer is lower than 0.5%, and relative viscosity is controlled at RV2.8-3.0 (96% vitriol oil).
The present invention further is set to: said step 7) also comprises: will behind the centrifuge dewatering of delivering to the drying tower top behind the rotary discharge valve, fall into drying tower through caprolactam after the step 6) extraction and the section of nylon salt multipolymer; Section is plunger flow from top to down in drying tower; High-purity cycling hot nitrogen divides top and bottom two-way to get into drying tower; Section stopped in drying tower 28 hours, and temperature is controlled between 122-112 ℃ in the drying tower.
Through adopting technique scheme, the top circulating nitrogen gas mainly is to the section heating and removes surface water that the bottom circulating nitrogen gas mainly is to remove the section internal moisture, guarantees that finally multipolymer section water cut is less than or equal to 500ppm.
Below in conjunction with accompanying drawing the present invention is further described.
Description of drawings
Fig. 1 is the used apparatus structure synoptic diagram of production technique of caprolactam of the present invention and the section of nylon salt multipolymer.
Embodiment
1), the preparation of raw material referring to accompanying drawing 1, the production technique of caprolactam disclosed by the invention and nylon salt multipolymer section may further comprise the steps:: the aqueous solution and the additive that prepare caprolactam melt, nylon salt respectively; 2), raw material that step 1) is made squeezes into mixing tank 1 and mixes, mixing tank 1 can be static mixer or dynamic hybrid chamber; 3), will be through step 2) the blended material gets into pre-polymerization tower 2; Caprolactam quickens open loop and carries out addition and part polycondensation respectively under the effect of water and nylon salt; Obtain the melt of low-molecular-weight caprolactam and nylon salt multipolymer, and in pre-polymerization tower 2, slough excessive moisture; 4) the low-molecular-weight caprolactam that, step 3) is made and the melt of nylon salt multipolymer are after film forming device 3 is sloughed residual water-content; Enter into post polymerization tower 4; Slough the low-molecular-weight caprolactam of moisture and the melt of nylon salt multipolymer and in post polymerization tower 4, carry out copolycondensation and balance, molecular weight is further brought up to the caprolactam of formation desired molecule amount and the melt of nylon salt multipolymer; 5) caprolactam that, step 4) is made and the melt of nylon salt multipolymer carry out pelletizing through dicing machine 5 and obtain caprolactam and cut into slices with the nylon salt multipolymer; 6) caprolactam and the section of nylon salt multipolymer that, step 5) are made extract; 7), will carry out drying through caprolactam after the step 6) extraction and nylon salt multipolymer section entering drying tower 6; 8), will get into cooling feed bin 7 through the section of the dried caprolactam of step 7) and nylon salt multipolymer cools off and obtains caprolactam and the nylon salt multipolymer finished product of cutting into slices.Through adopting technique scheme, caprolactam that makes and the section of nylon salt multipolymer are keeping nylon 6 its outstanding tensile strength, resistance to impact shock and the anti-intensity that pierces through; Good barrier properties for gases outside good thermotolerance, mist degree and glossiness and the good characteristics such as impressionability, has improved low-temperature performance simultaneously; Improved flexibility; Prevent food product pack in refrigerating process, packing film hardening, easy to be broken, and have higher transparency.
Present embodiment further is set to: the top in the pre-polymerization tower 2 of said step 3) is provided with tubulation; The arranged outside of pre-polymerization tower 2 has insulation jacket; Each is heated the tubulation of said pre-polymerization tower 2 and insulation jacket by one tunnel gas phase heating agent 201; Pressure in the pre-polymerization tower 2 between 1.5-2.5bar, in the pre-polymerization tower 2 temperature between 245-275 ℃, through step 2) the blended material got in the pre-polymerization tower 2 reservation 4 hours.Through adopting technique scheme; Caprolactam is under the effect of water and nylon salt; Open loop, addition and part polycondensation can be carried out smoothly, and the low-molecular-weight caprolactam in exit and the melt viscosity of nylon salt multipolymer are controlled at relative viscosity RV2.0-2.1 (96% vitriol oil).
Present embodiment further is set to: said step 4) also comprises: slough the low-molecular-weight caprolactam of moisture and the post polymerization tower 4 internal reaction 2-3s of melt between 260-265 ℃ hours of nylon salt multipolymer, make molecular weight further improve; Be provided with tubulation in the post polymerization tower 4; The tubulation of post polymerization tower 4 cools off through circulation heating agent 401 and removes reaction heat then; Make the insulation balance that material carried out 6-7 hour between 245-255 ℃; Make the molecular chain more even distribution through molecular chain exchange, and reach the caprolactam of desired molecule amount and the melt of nylon salt multipolymer.Through adopting technique scheme; The melt of low-molecular-weight caprolactam and nylon salt multipolymer can carry out copolycondensation and balance smoothly, and the melt viscosity of caprolactam and nylon salt multipolymer is controlled at relative viscosity RV2.6-2.8 (96% vitriol oil).
Present embodiment further is set to: said step 1) also comprises: with solid-state caprolactam through kibbler get into melting still 8 and through circulation transferpump 9 get into behind the interchanger 10 again through steam heating and with new solid material mixed melting, after strainer 11 smart filtrations, squeeze into a middle vessel 12 that presss from both sides hot water thermal insulating then with pump; Preparing tank 13 at jacketed and whisking appliance adds the hot de-salted water of deoxidation through under meter earlier; Be mixed with 66 salt brine solutions through being metered into solid-state nylon salt through stirring then with water; The preparation temperature is controlled between 75-100 ℃; The concentration of the aqueous solution is controlled at below 60%, and squeezes into the middle vessel 14 of band hot water thermal insulating.Through adopting technique scheme, make the subsequent production of caprolactam and nylon salt multipolymer section to carry out smoothly.
Present embodiment further is set to: raw material peace quality is 70-94.9% than caprolactam ratio said step 2), and 66 salt ratios are 30-5%, and additive is 0.05-0.2%.Through adopting technique scheme, make the subsequent production of caprolactam and nylon salt multipolymer section to carry out smoothly.
Present embodiment further is set to: said step 6) also comprises: caprolactam that step 5) is made and the section of nylon salt multipolymer divide dried up through drying machine and through being fed into extraction tower 14 behind the vibrosieve divorce particle; Preferably; Extract through three extraction towers 14; In the extraction tower 14 be normal pressure, be evenly distributed with a lot of cowling panels in the tower in case section from top to bottom, the de-ionized process water of heat is plunger flow from top to bottom, extraction tower 14 interior temperature are controlled between 98-110 ℃.Through adopting technique scheme; Make caprolactam monomer and oligopolymer in the section of caprolactam and nylon salt multipolymer carry out the water hot extraction; Low molecule content in caprolactam and the section of nylon salt multipolymer is lower than 0.5%, and relative viscosity is controlled at RV2.8-3.0 (96% vitriol oil).
Present embodiment further is set to: said step 7) also comprises: will after whizzer 16 dehydrations of delivering to drying tower 6 tops behind the rotary discharge valve 15, fall into drying tower 6 through caprolactam after the step 6) extraction and the section of nylon salt multipolymer; Section is plunger flow from top to down in drying tower 6; High-purity cycling hot nitrogen divides top and bottom two-way to get into drying tower 6; Section stopped in drying tower 28 hours, and temperature is controlled between 122-112 ℃ in the drying tower.Through adopting technique scheme, the top circulating nitrogen gas mainly is to the section heating and removes surface water that the bottom circulating nitrogen gas mainly is to remove the section internal moisture, guarantees that finally caprolactam and nylon salt multipolymer section water cut is less than or equal to 500ppm.Preferably, caprolactam that the cooling feed bin comes out and nylon salt multipolymer section finished product are delivered to finished product packing feed bin 18 through circulating nitrogen gas air-flow 17, and then measure and vacuum packaging.
Claims (7)
1), the preparation of raw material 1. the production technique of caprolactam and nylon salt multipolymer section is characterized in that: may further comprise the steps:: the aqueous solution and the additive that prepare caprolactam melt, nylon salt respectively; 2) raw material that, step 1) is made is squeezed into mixing tank and is mixed; 3), will be through step 2) the blended material gets into the pre-polymerization tower; Caprolactam quickens open loop and carries out addition and part polycondensation respectively under the effect of water and nylon salt; Obtain the melt of low-molecular-weight caprolactam and nylon salt multipolymer, and in the pre-polymerization tower, slough excessive moisture; 4) the low-molecular-weight caprolactam that, step 3) is made and the melt of nylon salt multipolymer are after film forming device is sloughed residual water-content; Enter into the post polymerization tower; Slough the low-molecular-weight caprolactam of moisture and the melt of nylon salt multipolymer and in the post polymerization tower, carry out copolycondensation and balance, molecular weight is further brought up to the caprolactam of formation desired molecule amount and the melt of nylon salt multipolymer; 5) caprolactam that, step 4) is made and the melt of nylon salt multipolymer carry out pelletizing through dicing machine and obtain caprolactam and cut into slices with the nylon salt multipolymer; 6) caprolactam and the section of nylon salt multipolymer that, step 5) are made extract; 7), will carry out drying through caprolactam after the step 6) extraction and nylon salt multipolymer section entering drying tower; 8), will get into the cooling feed bin through the section of the dried caprolactam of step 7) and nylon salt multipolymer cools off and obtains caprolactam and the nylon salt multipolymer finished product of cutting into slices.
2. the production technique of caprolactam according to claim 1 and the section of nylon salt multipolymer; It is characterized in that: the top in the pre-polymerization tower of said step 3) is provided with tubulation; The arranged outside of pre-polymerization tower has insulation jacket; Each is heated the tubulation of said pre-polymerization tower and insulation jacket by one tunnel gas phase heating agent; Pressure in the pre-polymerization tower between 1.5-2.5bar, in the pre-polymerization tower temperature between 245-275 ℃, through step 2) the blended material got in the pre-polymerization tower reservation 4 hours.
3. the production technique of caprolactam according to claim 1 and 2 and the section of nylon salt multipolymer; It is characterized in that: said step 4) also comprises: slough the post polymerization tower internal reaction of melt between 260-265 ℃ 2-3 hour of low-molecular-weight caprolactam and the nylon salt multipolymer of moisture, make molecular weight further improve; Be provided with tubulation in the post polymerization tower; The tubulation of post polymerization tower cools off through the circulation heating agent and removes reaction heat then; Make the insulation balance that material carried out 6-7 hour between 245-255 ℃; Make the molecular chain more even distribution through molecular chain exchange, and reach the caprolactam of desired molecule amount and the melt of nylon salt multipolymer.
4. the production technique of caprolactam according to claim 3 and the section of nylon salt multipolymer; It is characterized in that: said step 1) also comprises: with solid-state caprolactam through kibbler get into the melting still and through the circulation transferpump get into behind the interchanger again through steam heating and with new solid material mixed melting, squeeze into a middle vessel that presss from both sides hot water thermal insulating with pump after filtering through strainer is smart then; Preparing tank at jacketed and whisking appliance adds the hot de-salted water of deoxidation through under meter earlier; Be mixed with 66 salt brine solutions through being metered into solid-state nylon salt through stirring then with water; The preparation temperature is controlled between 75-100 ℃; The concentration of the aqueous solution is controlled at below 60%, and squeezes into the middle vessel of band hot water thermal insulating.
5. the production technique of caprolactam according to claim 4 and the section of nylon salt multipolymer is characterized in that: raw material peace quality is 70-94.9% than caprolactam ratio said step 2), and 66 salt ratios are 30-5%, and additive is 0.05-0.2%.
6. the production technique of caprolactam according to claim 5 and the section of nylon salt multipolymer; It is characterized in that: said step 6) also comprises: caprolactam that step 5) is made and the section of nylon salt multipolymer divide dried up through drying machine and through being fed into extraction tower behind the vibrosieve divorce particle; In the extraction tower is normal pressure; Be evenly distributed with a lot of cowling panels in the tower so as the section from top to bottom, heat the de-ionized process water be plunger flow from top to bottom; And caprolactam monomer and the oligopolymer in the multipolymer section carried out the water hot extraction, the interior temperature of extraction tower is controlled between 98-110 ℃.
7. the production technique of caprolactam according to claim 6 and the section of nylon salt multipolymer; It is characterized in that: said step 7) also comprises: will behind the centrifuge dewatering of delivering to the drying tower top behind the rotary discharge valve, fall into drying tower through caprolactam after the step 6) extraction and the section of nylon salt multipolymer; Section is plunger flow from top to down in drying tower; High-purity cycling hot nitrogen divides top and bottom two-way to get into drying tower; Section stopped in drying tower 28 hours, and temperature is controlled between 122-112 ℃ in the drying tower.
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