阅读说明：本技术 一种环保型尼龙6消光剂溶液的添加系统及工艺与尼龙6生产系统 (Addition system and process of environment-friendly nylon 6 delustering agent solution and nylon 6 production system ) 是由 袁甫荣 肖光 赵蒙 王延峰 谢培建 管艳华 王新 于 2020-06-30 设计创作，主要内容包括：本发明涉及一种环保型尼龙6消光剂溶液的添加系统及工艺与尼龙6生产系统,属于尼龙6生产领域,全程自动化,利用自动加料机自动加料,在线分析、离心分离。全程密闭化,采用密闭的离心机代替敞开式的沉降槽,防止杂物的混入。全程无废物产生,采用研磨机对回收的TiO<Sub>2</Sub>残渣进行研磨,进一步回收利用。其生产工艺主要包括溶剂的配制(己内酰胺水溶液的配制)、溶液的配制(配制和稀释)、残渣的回收利用等过程。(The invention relates to an environment-friendly nylon 6 flatting agent solution adding system and process and a nylon 6 production system, belongs to the field of nylon 6 production, is full-automatic, and utilizes an automatic feeding machine to automatically feed materials, perform online analysis and centrifugal separation. The whole process is sealed, and a sealed centrifuge is adopted to replace an open settling tank, so that impurities are prevented from being mixed. No waste is generated in the whole process, and a grinder is adopted to recycle the recycled TiO 2 The residue is ground and further recycled. The production process mainly comprises the preparation of solvent (caprolactam water solution) and solution (preparation)Preparation and dilution), and recycling of residues.)

1. An adding process of an environment-friendly nylon 6 flatting agent solution is characterized by comprising the following steps:

mixing liquid caprolactam with desalted water to form a caprolactam water solution;

mixing solid TiO₂Mixing with caprolactam water solution, diluting to obtain TiO₂Diluting the solution;

adding TiO into the mixture₂The diluted solution is centrifugally separated to obtain TiO₂Suspension and coarse phase TiO₂；

Subjecting the TiO to a reaction₂Diluting the suspension, detecting, filtering and storing for later use;

the coarse phase TiO₂Ground to obtain solid TiO₂And recycling.

2. The process for adding an environment-friendly nylon 6 matting agent solution according to claim 1, wherein the mass ratio of the liquid caprolactam to the desalted water is 7: 3 to 5.

3. The process of claim 1, wherein the solid TiO is added to the solution of nylon 6 matting agent₂The mass ratio of the caprolactam aqueous solution to the caprolactam aqueous solution is 1: 3 to 5.

4. The process of claim 1, wherein said TiO is added to a solution of a gloss reducing agent selected from the group consisting of nylon 6 and mixtures thereof₂The concentration of the diluent is 20-20.5%.

5. The process of claim 1, wherein said TiO is added to a solution of a gloss reducing agent selected from the group consisting of nylon 6 and mixtures thereof₂The suspension is diluted to the concentration of 15 to 15.5 percent.

6. The process of claim 1, wherein the coarse phase TiO is added into the solution of nylon 6 matting agent₂Grinding to a particle size of 0.8-1.2 μm.

7. An addition system of environment-friendly nylon 6 flatting agent solution is characterized by comprising: automatic feeder, TiO₂Mixing tank, TiO₂Dilution tank, centrifuge, TiO₂Suspension preparing tank, online analyzer and TiO₂Suspension filter, TiO₂Suspension tank, TiO₂Coarse phase groove, grinder, TiO₂A crude phase blending tank and a caprolactam water solution preparation tank; the automatic feeder and TiO₂Mixing tank, TiO₂Dilution tank, centrifuge, TiO₂Suspension adjustment tank and TiO₂Suspension pump, TiO₂Suspension filter, TiO₂The suspension storage tanks are connected in sequence, and the TiO is₂Suspension preparation tank and TiO₂A backflow pipeline is arranged between the suspension pumps, and an online analyzer is arranged on the backflow pipeline.

8. The system for adding an environmentally friendly nylon 6 matting agent solution according to claim 7 wherein the centrifugal pump is further in combination with TiO₂Coarse phase channel, TiO₂Coarse phase pump, grinder, TiO₂Coarse phase blending tank connected, the TiO₂The coarse phase blending tank is also mixed with TiO₂The mixing tanks are connected.

9. The system of claim 7, wherein said TiO is added to said solution of nylon 6 matting agent ₂Mixing tank, TiO₂Dilution tank, centrifuge, TiO₂Suspension adjustment tank and TiO₂The suspension storage tanks are respectively connected with a caprolactam water solution preparation tank.

10. A nylon 6 production system, comprising: an addition system of the environment-friendly nylon 6 matting agent solution described in any one of claims 7 to 9.

Technical Field

The invention belongs to the field of nylon 6 production, and relates to a nylon 6 delustering agent TiO₂And (5) solution prefabrication process.

Background

The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.

The main application of nylon 6 high-speed spinning is civil silk used in textile industry. High-speed spinning of nylon 6 by using TiO₂The light-transmitting agent is used as a flatting agent to shield the light transmission of the product so as to meet the requirement of the light transmission of the textile.

In the production process of nylon 6 high-speed spinning, TiO conventional in industry₂The solution prefabricating process includes natural settling in several parallelly connected square settling tanks, discharging the clear liquid to TiO₂The suspension is added into the system through a metering pump in a suspension storage tank. The process has low automation level, and can be used for manually feeding and analyzing concentration and TiO₂The residues are manually packed into bags for taking out after being dried in the air and cannot be recycled.

The process has the advantages that natural sedimentation is adopted for about 20 hours, the time is long, the automation level is low, open type batching is realized, residues are not recycled, the labor and the time are wasted, the environment is not protected, and the risk that sundries fall into the open type batching to influence the product quality is also existed.

Disclosure of Invention

In order to overcome the problems, the invention provides an environment-friendly TiO 6 delustering agent of nylon 6₂And (5) solution prefabrication process. The automatic level is high, automatic material conveying, online concentration analysis, automatic material returning, and manpower resources are saved.

In order to achieve the technical purpose, the invention adopts the following technical scheme:

The invention provides an adding process of an environment-friendly nylon 6 flatting agent solution, which comprises the following steps:

mixing liquid caprolactam with desalted water to form a caprolactam water solution;

mixing solid TiO₂Mixing with caprolactam water solution, diluting to obtain TiO₂Diluting the solution;

adding TiO into the mixture₂The diluted solution is centrifugally separated to obtain TiO₂Suspension and coarse phase TiO₂；

Subjecting the TiO to a reaction₂Diluting the suspension, detecting, filtering and storing for later use;

the coarse phase TiO₂Ground to obtain solid TiO₂And recycling.

Existing centrifugal titanium dioxide suspension production systems typically employ open or overhead tanks with vents. Therefore, the invention designs the closed mixing tank, which can well prevent dust and other impurities from falling in, the quality of the matting agent is better, and the product is matt without fouling. The concentration is automatically analyzed, the automatic adjustment is realized, the hysteresis adjustment phenomenon of manual analysis is eliminated, and the product is more stable.

In a second aspect of the present invention, there is provided an adding system of an environment-friendly nylon 6 matting agent solution, comprising: automatic feeder, TiO₂Mixing tank, TiO₂Dilution tank, centrifuge, TiO₂Suspension preparing tank, online analyzer and TiO₂Suspension filter, TiO ₂Suspension tank, TiO₂Coarse phase groove, grinder, TiO₂A crude phase blending tank and a caprolactam water solution preparation tank; the automatic feeder and TiO₂Mixing tank, TiO₂Dilution tank, centrifuge, TiO₂Suspension adjustment tank and TiO₂Suspension pump, TiO₂Suspension filter, TiO₂The suspension storage tanks are connected in sequence, and the TiO is₂Suspension preparation tank and TiO₂A backflow pipeline is arranged between the suspension pumps, and an online analyzer is arranged on the backflow pipeline.

Compared with the open design, the designPlacing closed TiO₂The mixing tank needs to set the normal pressure equipment as a pressure container, namely, the upper top is designed to be a sealing type instead of a flat top or an open type. Therefore, the invention arranges the breather valve on the tank top and arranges the nitrogen seal protection at the same time, thereby preventing impurities from falling into the tank and preventing the mixed liquid from contacting with oxygen to generate oxidation reaction and ensuring the stable reaction.

In a third aspect of the present invention, there is provided a nylon 6 production system comprising: any one of the above-mentioned systems for adding an environmentally friendly nylon 6 matting agent solution.

Existing technology for preparing TiO by centrifugal separation₂The solution needs 3 hours, and the original process utilizes a settling tank to naturally settle to prepare TiO₂Solution, taking 20 hours, greatly shortened TiO₂Preparation time of the solution.

The invention has the beneficial effects that:

(1) residue TiO is ground by a grinder₂And the treatment and recycling are carried out, so that the environment-friendly production is realized.

(2) The automatic level is high, automatic material conveying, online concentration analysis, automatic material returning, and manpower resources are saved.

(3) Existing technology for preparing TiO by centrifugal separation₂The solution needs 3 hours, and the original process utilizes a settling tank to naturally settle to prepare TiO₂Solution, taking 20 hours, greatly shortened TiO₂Preparation time of the solution.

(4) And a closed system is adopted, so that the influence of impurities mixed in the process on the product quality is avoided.

(5) The method is simple, low in cost, strong in practicability and easy to popularize.

Drawings

The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.

FIG. 1 shows Nylon hexaTiO of example 1 of the present invention₂The preparation process route of the additive is shown schematically.

Wherein: 1. automatic feeder, 2.TiO₂Mixing tank, 3. dispersion pump、4.TiO₂Dilution tank, 5.TiO₂Delivery pump, 6. centrifuge, 7.TiO₂Suspension preparation tank, 8.TiO₂Suspension pump, 9. on-line analyzer, 10.TiO₂Suspension filter, 11.TiO ₂Stock tank for suspension, 12.TiO₂Coarse phase channel, 13.TiO₂Coarse phase pump, 14. mill, 15.TiO₂A crude phase preparation tank and a caprolactam water solution preparation tank.

FIG. 2 is a schematic representation of a closed TiO of the present invention₂The structure of the mixing tank is schematically shown, wherein, 18 breather valves and 19 nitrogen seals are arranged.

Detailed Description

It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.

It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.

Environment-friendly nylon 6TiO₂The solution prefabricating process is full-automatic, automatic feeding is carried out by an automatic feeding machine, and online analysis and centrifugal separation are carried out. The whole process is sealed, and a sealed centrifuge is adopted to replace an open settling tank, so that impurities are prevented from being mixed. No waste is generated in the whole process, and a grinder is adopted to recycle the recycled TiO ₂The residue is ground and further recycled.

The production process mainly comprises the preparation of a solvent (the preparation of a caprolactam water solution), the preparation of a solution (the preparation and dilution), and the recycling of residues, and comprises the following specific processes:

(1) preparing a caprolactam water solution: liquid caprolactam and desalted water are injected into the upper part of a caprolactam water solution preparation tank in a chain manner according to the mass ratio of 7:3 by a metering pump. After mixing, the mixture is conveyed to the lower part of a caprolactam water solution preparation tank through a pipeline in the tank.

(2)TiO₂Preparing a solution: solid TiO₂The materials are added into the TiO through an automatic feeder₂Injecting the prepared caprolactam water solution into the TiO in the mixing tank₂In a mixing tank. The mass ratio of the two is 1:3, the mixed solution is discharged into TiO after being circularly dispersed for a period of time by a dispersion pump₂Diluting in a dilution tank.

(3)TiO₂Diluting a mixed solution: to TiO 2₂The aqueous solution of caprolactam is injected into the dilution tank to make TiO₂The concentration is diluted from 25% to 20%.

(4)TiO₂And (3) centrifugal separation of the mixed solution: diluting the diluted TiO₂The mixed solution passes through TiO₂Pumping the TiO into a centrifuge by a delivery pump to separate out TiO₂The suspension is discharged into TiO₂Suspension preparation tank. TiO 2₂Discharging the residue into TiO₂And (4) a coarse phase groove.

(5)TiO₂And (3) preparing and storing the suspension: to TiO 2 ₂Injecting caprolactam water solution into the blending tank to enable TiO₂The suspension concentration is diluted from 20% to 15%. TiO 2₂The suspension is passed over TiO₂An on-line concentration analyzer of a reflux pipeline of the suspension pump is used for analyzing qualified TiO₂The suspension being pumped through the TiO₂The suspension is filtered by a suspension filter and then discharged into TiO₂Storage tanks for suspensions, TiO₂And finishing the preparation of the additive.

(6) Coarse phase TiO₂Grinding: coarse phase TiO₂From TiO₂Pumping the coarse phase into a grinding machine, grinding the coarse phase until the average particle size is about 1 micron, and adding the coarse phase into TiO₂Crude phase preparation tank and then conveying to TiO₂And (5) recycling in the mixing tank.

Environment-friendly nylon 6TiO₂The main production process of the pre-preparation process of the flatting agent comprises solvent preparation, solution preparation and residue recovery.

The main equipment comprises an automatic feeder and TiO₂A mixing tank, a dispersion pump,TiO₂Dilution tank, TiO₂Transfer pump, centrifuge, TiO₂Suspension adjustment tank and TiO₂Suspension pump, on-line analyzer, TiO₂Suspension filter, TiO₂Suspension tank, TiO₂Coarse phase channel, TiO₂Coarse phase pump, grinder, TiO₂A crude phase preparation tank and a caprolactam water solution preparation tank.

The main production process comprises the following steps:

(1) preparing a caprolactam water solution: injecting liquid caprolactam and desalted water into the upper part of a caprolactam water solution preparation tank according to the mass ratio of 7: 3. After mixing, the mixture is discharged to the lower part of a caprolactam water solution preparation tank through a pipeline.

(2)TiO₂Preparing a mixed solution: ton-coated solid TiO₂Added to TiO by an automatic feeder₂Injecting the prepared caprolactam water solution into the TiO in the mixing tank₂In a mixing tank. The mass ratio of the two is 1:3, and after the dispersion pump disperses for a period of time, the mixed solution is discharged into TiO₂Diluting in a dilution tank.

(3)TiO₂Diluting a mixed solution: to TiO 2₂The aqueous solution of caprolactam is injected into the dilution tank to make TiO₂The concentration is diluted from 25% to 20%.

(4)TiO₂And (3) centrifugal separation of the mixed solution: diluting the diluted TiO₂The mixed solution passes through TiO₂Pumping the TiO into a centrifuge by a delivery pump, separating for a period of time, and separating out the TiO₂The suspension is discharged into TiO₂Suspension preparation tank. Coarse phase TiO₂To TiO₂And (4) a coarse phase groove.

(5)TiO₂And (3) preparing and storing the suspension: to TiO 2₂Injecting caprolactam water solution into the blending tank to enable TiO₂Suspension concentration is diluted from 20% to 15%₂The suspension is passed over TiO₂An on-line concentration analyzer of a reflux pipeline of the suspension pump is used for analyzing qualified TiO₂The suspension being pumped through the TiO₂The suspension is filtered by a suspension filter and then discharged into TiO₂Storage tanks for suspensions, TiO₂And finishing the preparation of the additive.

(6) Coarse phaseTiO₂Grinding: coarse phase TiO₂From TiO₂Pumping the coarse phase into a grinder, grinding the coarse phase until the average particle size is 1 micron and entering TiO₂A coarse phase preparation tank is arranged and then discharged into TiO ₂And (5) recycling in the mixing tank.

In some embodiments, the container device is installed in each floor through the ear-type support, the height of each floor is about 7m, the installation is convenient, and the whole structure of the device is stable.

In some embodiments, the TiO₂Mixing tank, TiO₂Dilution tank, TiO₂Suspension preparation tank, TiO₂Suspension tank, TiO₂Coarse phase channel, TiO₂The coarse phase blending tank is internally provided with stirring, and the external part of the coarse phase blending tank is wound by a half pipe, wherein TiO₂The mixing tank is filled with cooling water in the half pipes at about 6 deg.c and the other half pipes at about 30 deg.c for homogeneous mixing and easy temperature control.

In some embodiments, the caprolactam water solution preparation tank is divided into two parts by a partition plate, an upper inner coil pipe is filled with chilled water, a lower inner coil pipe is filled with cooling water, and an upper part and a lower part are connected by a pipeline with a quick-cutting valve.

In some embodiments, the TiO₂Suspension filter and TiO₂The filter core structure of the filter is absorbent cotton with a 316L framework, and the filtering precision is 1 mu m, so that the filtering effect is ensured, and the quality of the matting agent is improved.

In some embodiments, the coarse phase purge used by the centrifuge is an aqueous caprolactam solution. The centrifuge of the invention adopts a washing machine-like centrifuge with a filter bag, and the suspension is thrown out of the storage tank. The crude phase is intermittently withdrawn from the bottom. Due to the continuous centrifugal discharge, it is more efficient than overflow collection.

In the existing centrifugal titanium dioxide suspension liquid preparation system, because the material mixing effect is poor, a dispersing agent needs to be added, but if the dispersing agent is added, more small-particle materials influence the wire drawing of a nylon 6 product, and the wire breakage is easy to occur, therefore, in some embodiments, the automatic feeding machine is a weight-loss type constant feeder,the model is ICS-LW-6 manufacturer: wu hong Hui electronics Ltd. TiO of the invention₂The adding mode is a spiral automatic feeder, and the caprolactam adding mode is a jet self-mixing adding mode, namely: a plurality of injection holes with the aperture of 10-20 μm, preferably 4, are arranged at the feed inlet. The research finds that: through the mutual cooperation of the local negative pressure that above-mentioned spiral feed and jet mixing formed, increase liquid axial mixing process, make the fluid can reach high-efficient the mixture, satisfied the misce bene of material, consequently, need not to add dispersant again, and product quality obtains effectively promoting.

The present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.