CN112694652B

CN112694652B - Preparation method of watertight connector, product of watertight connector and composite rubber material for preparing watertight connector

Info

Publication number: CN112694652B
Application number: CN202011500979.0A
Authority: CN
Inventors: 胡奇志; 黄永强
Original assignee: Beijing Haidichuang Technology Co ltd; CSSC Systems Engineering Research Institute
Current assignee: Beijing Haidichuang Technology Co ltd; CSSC Systems Engineering Research Institute
Priority date: 2020-12-17
Filing date: 2020-12-17
Publication date: 2022-12-09
Anticipated expiration: 2040-12-17
Also published as: CN112694652A

Abstract

The invention relates to the field of watertight devices, in particular to a preparation method of a watertight connector, a product of the watertight connector and a composite rubber material for preparing the watertight connector. The preparation method of the watertight connector comprises the following steps: preparing a composite rubber material and forming the watertight connector. The watertight connector has good water tightness, insulativity and pressure resistance, meets the current deep sea coverage, and meets the requirement of stable electric transmission use.

Description

Preparation method of watertight connector, product thereof and composite rubber material for preparing watertight connector

Technical Field

The invention relates to the field of watertight devices, in particular to a preparation method of a watertight connector, a product of the watertight connector and a composite rubber material for preparing the watertight connector.

Background

Watertight connectors are also known as watertight connectors. As one of the important parts of the normal operation of underwater equipment, at present, the application range of the watertight connector is quite wide, and the watertight connector comprises the fields of underwater engineering machinery, operating instruments, underwater illumination, underwater power distribution systems, diving assembly devices, ocean oil production platforms, ocean bottom observation networks and the like.

Because the development and the start of the watertight connector in China are late, the technology has a quite large gap with that of the watertight connector in Western, the problems of no fixed model series, unstable process flow, incapability of reaching the production level, no standardized detection rule, no universal technical specification and the like exist in the product, and the defects cause the problems of the existing watertight connector product in China in the aspects of technical specification standardization, product performance stability, mass production capacity and the like. Therefore, at present, most of deep sea common products in China depend on imports, which seriously restricts the development of deep sea technology in China. On the other hand, breaking through the monopoly of foreign technologies, realizing product alternative import and reducing investment cost is also very urgent.

How to ensure the watertight performance, the insulating performance and the pressure resistance of the rubber body watertight connector when working in a deep sea environment is a technical difficulty, and in addition, the connector is in a severe deep sea environment for a long time, so that the connector is difficult to connect reliably for a long time and maintain. During underwater operation, the watertight connector must be able to maintain the electrical performance normally and the mechanical connection reliably, resistant to seawater corrosion, good watertight and resistant to water pressure. In case of failure of the plug assembly connected with the cable, the reliability of sealing between connector bases must be ensured, so that the safety of internal equipment is ensured, and external high-water-pressure seawater is never allowed to enter the equipment cabin through the connector. Therefore, the tightness becomes a key index for verifying a watertight connector product, and the sealing between the connector plug and the socket must be ensured; sealing between the connector and the fixed panel; sealing between the connector and the mating cable.

In view of the above, the present invention is particularly proposed.

Disclosure of Invention

The invention aims to provide a method for preparing a watertight connector.

The second invention of the invention aims to provide the watertight connector prepared by the method.

The third invention of the present invention is to provide a composite rubber material.

The fourth invention of the invention aims at providing the application of the composite rubber material.

In order to realize the purpose of the invention, the technical scheme is as follows:

the invention provides a preparation method of a watertight connector, which at least comprises the following steps:

s1, preparing a composite rubber material; the raw materials of the composite rubber material comprise: 79.5 to 80.5 portions of chloroprene rubber, 34.5 to 35.5 portions of tackifying master batch, 0.95 to 1.05 portions of insoluble sulfur, 4.7 to 5.2 portions of zinc oxide, 34 to 36 portions of modified talcum powder, 3 to 5 portions of magnesium oxide, 0.5 to 1.5 portions of anti-aging agent, 0.5 to 1.5 portions of processing aid and 1.5 to 2.5 portions of accelerator; the tackifying master batch comprises 20 parts by weight of chloroprene rubber, 8-12 parts by weight of terpene resin and 3-7 parts by weight of modified talcum powder; the raw materials of the composite rubber material are preferably as follows: 80 parts of chloroprene rubber, 35 parts of tackifying master batch, 35 parts of modified talcum powder, 1 part of insoluble sulfur, 5 parts of zinc oxide, 4 parts of magnesium oxide, 1 part of anti-aging agent, 2 parts of stearic acid and 2 parts of accelerator; the tackifying master batch preferably comprises the following components: 20 parts of chloroprene rubber, 8-10 parts of terpene resin and 5 parts of modified talcum powder;

s2, molding of the watertight connector: pretreating accessories of the watertight connector, assembling a mould and the accessories, preheating the rubber compound, injecting glue, vulcanizing, and performing aftertreatment to obtain the watertight connector;

the pressure of the glue injection is 10-12KN.

Optionally, the raw material of the composite rubber material further comprises carbon black, preferably carbon black N330, more preferably the addition amount of the carbon black is 0.45-0.55 part by weight, more preferably 0.5 part by weight;

and/or said neoprene is selected from neoprene Baypren711;

and/or the accelerator is selected from N, N' -dibutyl thiourea;

and/or the anti-aging agent is 4020NA;

and/or the processing aid is selected from stearic acid.

Optionally, the watertight connector includes a male connector and a female connector, the fitting of the male connector includes a needle core, an electrical conductor, a positioning needle, a copper housing and a rubber enclosure, and the fitting of the female connector includes an electrical conductor jack, a cable and a rubber enclosure;

the fittings of the pretreatment watertight connector comprise electric wire and stylet pretreatment and positioning needle pretreatment;

the assembly mold and the fitting include: and assembling the accessory of the male head in the preheated male head mould, and assembling the accessory of the female head in the preheated female head mould.

Optionally, the wire and stylet pretreatment comprises: cutting an electric wire, removing a cover of the electric wire, welding the electric wire and the stylet, and carrying out surface treatment on the stylet;

the surface treatment of the stylet comprises: and coating the part, which is used for being matched with the conductive jack of the female head, of the top of the needle core, coating glue on the position, to be injected with glue, of the needle core, and removing a coating.

Optionally, the preheating of the mold includes: and (3) putting the male die, the female die and the glue injection cylinder into an oven at 80 ℃, setting the temperature of a press to be 140 ℃, and preheating for 1 hour in advance.

Optionally, the preheating of the composite rubber material comprises: preparing the composite rubber material into a film with the thickness of 1-2mm, weighing 15-16g of the film after the die and the accessory are assembled, putting the film into a baking oven with the temperature of 75-85 ℃, and preheating for 2.5-3.0min.

Optionally, in the glue injection process, when the reading reduction rate of the pressure sensor is less than 20N/s, the glue injection is completed;

and/or in the glue injection process, a gradual injection and pressing mode is adopted; the pressing rate was 10KN/min.

And/or, when the pressure is lower than 10KN, the loading jack is used for pressurizing.

And/or the vulcanization condition is treatment at 140 ℃ for 40min;

and/or the post-treatment comprises demolding and sample surface treatment;

and/or the post-processing of the male head also comprises tail encapsulation.

The invention also relates to a watertight connector prepared by the preparation method.

The invention also relates to a composite rubber material which is prepared from the following raw materials: 80 parts of chloroprene rubber, 35 parts of tackifying master batch, 34-36 parts of modified talcum powder, 1 part of insoluble sulfur, 5 parts of zinc oxide, 3-5 parts of magnesium oxide, 0.5-1.5 parts of anti-aging agent, 0.5-1.5 parts of stearic acid and 1.5-2.5 parts of accelerator; the tackifying master batch comprises 20 parts by weight of chloroprene rubber, 8-12 parts by weight of terpene resin and 3-7 parts by weight of modified talcum powder;

the raw materials of the composite rubber material are preferably as follows: 80 parts of chloroprene rubber, 35 parts of tackifying master batch, 35 parts of modified talcum powder, 1 part of insoluble sulfur, 5 parts of zinc oxide, 4 parts of magnesium oxide, 1 part of anti-aging agent, 2 parts of stearic acid and 2 parts of accelerator; the tackifying master batch preferably comprises the following components: 20 parts of chloroprene rubber, 8-10 parts of terpene resin and 5 parts of modified talcum powder;

and/or the raw materials of the composite rubber material also comprise carbon black, preferably carbon black N330, and more preferably the addition amount of the carbon black is 0.5 part;

and/or said neoprene is selected from neoprene Baypren711;

and/or the accelerator is selected from N, N' -dibutyl thiourea;

and/or the anti-aging agent is 4020NA.

The invention also relates to the application of the composite rubber material in the preparation of a watertight device; optionally, when the composite rubber material is used for preparing the watertight device, the pressure during glue injection is 10-12KN.

The invention has at least the following beneficial effects:

the watertight connector has good water tightness, insulativity and pressure resistance, particularly has good water pressure resistance, meets the current deep sea coverage, and meets the stable electric transmission use requirement.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Furthermore, in the following detailed description, numerous specific details are set forth in order to provide a better understanding of the present invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In some instances, materials, components, methods, procedures, and the like that are well known to those of skill in the art have not been described in detail so as not to obscure the present invention.

Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations such as "comprises" or "comprising", etc., will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.

The embodiment of the invention relates to a preparation method of a watertight connector, which comprises two major parts, wherein one part is the preparation of a composite rubber material, and the other part is the molding of the watertight connector. The method comprises the steps of banburying and mixing raw materials to obtain mixed chloroprene rubber, and then preprocessing wires and cables, putting the wires and the cables into a mold and vulcanizing the wires and the cables. Therefore, the preparation method has the characteristic of simple preparation process and is convenient for practical popularization.

Specifically, the raw materials of the composite rubber material of the embodiment of the invention comprise: chloroprene rubber, tackifying master batch 3, modified talcum powder, insoluble sulfur, zinc oxide, magnesium oxide, an anti-aging agent, a processing aid and an accelerator; the tackifying master batch comprises chloroprene rubber, terpene resin and talcum powder.

The chloroprene rubber has good physical and mechanical properties, and is resistant to oil, heat, flame, sunlight, ozone, acid, alkali and chemical reagents. The disadvantages are poor cold resistance and storage stability. Has high tensile strength, elongation and reversible crystallinity, and good adhesion. The weather resistance and the ozone aging resistance are second to those of ethylene propylene rubber and butyl rubber. The heat resistance is equivalent to that of nitrile rubber, the decomposition temperature is 230-260 ℃, the rubber can resist 120-150 ℃ in a short term, the rubber can be used for a long term at 80-100 ℃, and the rubber has certain flame retardance. The oil resistance is second only to nitrile rubber. Good inorganic acid and alkali corrosion resistance. The cold resistance is slightly poor and the electrical insulation is poor. The raw rubber has poor storage stability, the phenomenon of 'self-vulcanization' can be generated, the Mooney viscosity is increased, and the raw rubber is hardened. According to research of the embodiment of the invention, chloroprene rubber is adopted as the matrix rubber material in the embodiment of the invention, and the tackifying master batch, the reinforcing agent, the cross-linking agent and the activating agent are matched to prepare the composite rubber material which has better fluidity and compressive capacity and can meet deep-water operation.

Specifically, the neoprene rubber of the embodiment of the invention adopts Baypren711 neoprene rubber products provided by Langshen company. The first digit indicates the tendency to crystallize, 1 mild, 2 moderate, 3 strong crystals; sulfur content, 5 low sulfur, 6 medium, 7 high sulfur. The second digit indicates the mooney viscosity, 1 low mooney, 2 moderate mooney, 3 high mooney. The third digit indicates the special property, and 1 indicates that the Mooney viscosity and the crystallization tendency of the raw rubber are low. Baypren711 has high sulfur content, good rubber material manufacturability, good adhesion with reinforced materials and wear resistance. A large number of screening tests show that the neoprene with the grade has the best comprehensive performance.

In the embodiment of the invention, the formula of the tackifying master batch is as follows: 20 parts of chloroprene rubber, 8-12 parts of terpene resin and 3-7 parts of modified talcum powder; preferably: 20 parts of neoprene, 8-10 parts of terpene resin and 5 parts of modified talcum powder, and mainly has the functions of increasing the adhesion between a rubber matrix and metal and keeping good sealing effect in water. By adding the tackifying master batch, the bonding strength between rubber and metal and the bonding strength between the cable outer insulating layer and the connector can be increased, and the insulating property and the pressure resistance of the product are not influenced. If the addition amount of the tackifying master batch is too large, the needle core part easily enters rubber materials in the molding process, and the contact resistance is influenced; if the amount is too small, the adhesive strength is insufficient.

The cross-linking agent has the main function of cross-linking raw chloroprene rubber, so that the mechanical property of the chloroprene rubber can be improved, and the chloroprene rubber has better pressure resistance. Specifically, insoluble sulfur may be used as the crosslinking agent. The insoluble sulfur can improve the rebound rate of the rubber product after being pressed. The addition amount of the insoluble sulfur is 0.95 to 1.05 parts by weight, preferably 1 part by weight, to 80 parts by weight of the chloroprene rubber. If the addition amount of the cross-linking agent is too large, the toughness of the rubber material is reduced, and the product is easy to tear; if the amount of addition is too small, the strength of the material becomes too low, and the sealing properties are poor.

The composite rubber material provided by the embodiment of the invention is further added with the reinforcing agent, and the embodiment of the invention specifically selects the modified talcum powder as the reinforcing agent of the chloroprene rubber, so that the composite rubber material has certain advantages of improving 100% stress at definite elongation of vulcanized rubber. The processing property and tensile strength of the rubber material added with the modified talcum powder are equivalent to those of the rubber material added with the carbon black N990, and the 300 percent stress at definite elongation and the tearing strength are slightly lower. Meanwhile, the talcum powder can improve the insulativity of the rubber product. The modified talcum powder can partially replace carbon black, and cannot cause excessive influence on the comprehensive performance of the rubber material. Meanwhile, the talcum powder is low in price, and the talcum powder is used for partially replacing carbon black, so that the cost can be reduced, and the product competitiveness can be improved. 34 to 36 parts by weight, preferably 35 parts by weight of chloroprene rubber added in an amount of 80 parts by weight; if the amount of the modified talc powder added is too large, the fluidity is adversely affected, and if the amount is too small, the insulation performance cannot be ensured.

The modified talcum powder is prepared by performing surface treatment on talcum powder by using a silane coupling agent KH570, wherein the surface treatment process comprises the steps of putting the talcum powder into 10 mass percent of KH570 alcohol solution, stirring for 30min, filtering, and drying the talcum powder in an oven at 80 ℃ for 36 hours. The composite rubber material provided by the embodiment of the invention is also added with zinc oxide and magnesium oxide, which are used as activating agents, and the zinc oxide and the magnesium oxide are used in a matching manner to catalyze and activate sulfur, so that the activity of the accelerator is higher. The zinc oxide is added in an amount of 4.7 to 5.2 parts by weight, preferably 5 parts by weight to 80 parts by weight of the chloroprene rubber, and the magnesium oxide is added in an amount of 3 to 5 parts by weight, preferably 4 parts by weight to 80 parts by weight of the chloroprene rubber. If the addition amount of the zinc oxide and the magnesium oxide is too large, the crosslinking degree of the product is too high, and the product is easy to tear; if the amount is too small, the strength of the product is lowered.

If the safety of rubber mixing is improved, active magnesium oxide and active zinc oxide can be used for replacing magnesium oxide and zinc oxide.

The composite rubber material provided by the embodiment of the invention is also added with an anti-aging agent, and the anti-aging agent is used for improving the aging performance of the material. The anti-aging agent is selected from 4020NA, and the anti-aging agent is added into 80 parts by weight of chloroprene rubber in an amount of 0.5-1.5 parts by weight, preferably 1 part by weight. If the amount of the antioxidant added is too large, the effect of the crosslinking system is adversely affected, and if the amount is too small, the protective effect is poor.

The processing aid of the composite rubber material provided by the embodiment of the invention is used for improving the stability of mechanical properties of chloroprene rubber and improving the distribution uniformity of a cross-linking agent, especially sulfur, in matrix rubber, and stearic acid is selected as the processing aid provided by the embodiment of the invention through a screening test. The amount of the chloroprene rubber added is 0.5 to 1.5 parts by weight, preferably 1 part by weight to 80 parts by weight of the chloroprene rubber. If the addition amount of the processing aid is too large, the bonding performance of the material is influenced, and if the addition amount is too small, the roller is easy to stick in the rubber mixing process.

The composite rubber material provided by the embodiment of the invention is also added with a rubber accelerator DBTU (totally named as N, N' -di-N-butylthiourea), which is commonly used as an accelerator of chloroprene rubber and is also an antiozonant of chloroprene rubber, and has the characteristics of no pollution and no discoloration. The amount of the chloroprene rubber added is 80 parts by weight, and the amount is 1.5 to 2.5 parts by weight, preferably 2 parts by weight. The addition of DBTU also contributes to the increase in the post-press rebound resilience of the rubber article. If the addition amount of the DBTU is too large, the material is high in brittleness and easy to tear; if the addition amount is too small, the elasticity of the material is poor, and the sealing property of the product is poor.

The composite rubber material of the embodiment of the invention is further added with carbon black as a coloring agent, preferably carbon black N330. The amount of the chloroprene rubber added is 0.45 to 0.55 part by weight, preferably 0.5 part by weight to 80 parts by weight. If the amount of carbon black added is too large, the insulation properties of the product are deteriorated, and if the amount added is too small, the dyeing is not uniform.

The formula of the composite rubber material of the embodiment of the invention is preferably as follows: 80 parts of chloroprene rubber, 35 parts of tackifying master batch, 35 parts of modified talcum powder, 1 part of insoluble sulfur, 5 parts of zinc oxide, 4 parts of magnesium oxide, 1 part of anti-aging agent, 2 parts of stearic acid and 2 parts of accelerator.

The preparation method of the composite rubber material provided by the embodiment of the invention can adopt a mixing process and mixing equipment commonly used in the current rubber processing process, so that the compounding agents such as the cross-linking agent, the reinforcing agent, the processing aid and the like can be completely and uniformly dispersed in the chloroprene rubber, and the composition of the composite rubber material is ensured to be uniform and consistent. The method specifically comprises the following steps: adding chloroprene rubber into an internal mixer, sequentially adding a tackifying master batch, stearic acid and an anti-aging agent, adding magnesium oxide, adding carbon black and modified talcum powder for three times, adding zinc oxide, sulfur and an accelerator, discharging after mixing, discharging by using an open mill, adjusting the roll distance of the open mill to be below 1mm, uniformly mixing for 5 times, then adjusting the roll distance, discharging and discharging to obtain the composite rubber material.

The watertight connector further comprises a molding step, wherein the watertight connector comprises a male head and a female head, accessories of the male head comprise a needle core, an electric lead, a positioning needle, a copper shell and a rubber wrapping body, accessories of the female head comprise a conductive jack, a cable and a rubber wrapping body, and the needle core is matched with the conductive jack for use.

The preparation method specifically comprises the following steps:

1. fitting of pre-treated watertight connector:

1.1 pretreating the wire and the needle core; cutting the electric wire, removing a cover of the electric wire, welding the electric wire and the needle core, and performing surface treatment on the needle core;

the surface treatment of the stylet comprises: and coating the part, matched with the conductive jack of the female head, of the top of the needle core, coating glue at the position, to be injected, on the needle core, and removing a coating. Can prevent pollution in the subsequent gluing process.

1.2, preprocessing a positioning needle;

2. an assembly mold and fitting comprising: assembling a male fitting in the preheated male die, and assembling a female fitting in the preheated female die;

the mould preheats and includes: and (3) putting the male die, the female die and the glue injection cylinder into an oven at 80 ℃, setting the temperature of a press to be 140 ℃, and preheating for 1 hour in advance.

3. Preheating the composite rubber material and injecting glue;

3.1 preheating the composite rubber material comprises the following steps: the composite rubber material is made into a film with the thickness of 1-2mm, after the assembly of the die and the accessory is finished, 15-16g of the film is weighed and placed in a baking oven with the temperature of 75-85 ℃ for preheating for 3min.

3.2, glue injection: the pressure is 10-12KN. The formula of the composite rubber material is matched with the glue injection pressure, and the working pressure of the prepared watertight connector can reach 60Mpa. In the glue injection process, a gradual injection and compression mode is adopted, and the compression rate is 10KN/min; in the glue injection process, the pressure can be slowly reduced, and when the pressure is lower than 10KN, the jack is loaded for pressure compensation. And when the dropping rate of the glue injection pressure is less than 20N/s, the glue injection is finished.

4. Vulcanizing, wherein the vulcanizing condition is that the vulcanizing is carried out for 40min at 140 ℃;

5. and post-processing, including demolding and sample surface treatment, and tail packaging.

Specifically, the male connector molding process comprises the following steps: the method comprises the steps of wire and stylet pretreatment (removing a wire cover, welding a wire and a stylet, and carrying out stylet surface treatment), positioning stylet pretreatment, mold preheating, mold assembly, composite rubber material preheating, injection molding (assembling an injection molding device, injection molding and disassembly), vulcanization, mold stripping, sample surface treatment and tail encapsulation. And performing the operations to obtain the male connector. The specific process conditions are detailed in example 2.

The connector female head forming process comprises the following steps: the method comprises the following steps of cable pretreatment (cutting, cable cover removing, needle core welding, needle core surface treatment, cable surface treatment and raw material tape winding), mold and press preheating, mold assembling, composite rubber material preheating, injection molding (assembling an injection molding device, injection molding and disassembling), vulcanization, mold stripping and sample surface treatment. And performing the operation to obtain the connector female head. The specific process conditions are detailed in example 3.

The embodiment of the invention relates to a watertight connector prepared by the preparation method. The watertight connector meets the organic connection of a watertight transmission assembly, can guarantee the long-time pressure-resistant sealing capacity of a sealing position while guaranteeing the mechanical strength, has higher reliability and safety, meets the current deep sea coverage, and meets the stable electric transmission use requirement.

The embodiment of the invention also relates to a composite rubber material, which is specifically described above. The composite rubber material of the invention can ensure that the watertight connector has good water tightness and good mechanical property, in particular to water pressure resistance.

The embodiment of the invention also relates to the application of the composite rubber material in the preparation of a watertight device; optionally, when the watertight device is prepared by using the composite rubber material, the pressure during glue injection is 10-12KN.

Example 1

The chloroprene rubber mixing process comprises the steps of preparing chloroprene rubber according to the formula shown in Table 1.

TABLE 1 formulation of Neoprene

According to the proportion, chloroprene rubber Baypren711 is added into an internal mixer, processing aids such as tackifying master batch, stearic acid, anti-aging agent and the like are sequentially added, magnesium oxide is added, carbon black and modified talcum powder are added in batches, and zinc oxide, sulfur and an accelerator DBTU are added. After the rubber material is mixed, discharging materials and discharging sheets by using an open mill. Adjusting the roll spacing of the open mill to be minimum, thinning for 5 times, gradually adjusting the roll spacing, discharging, blanking, stopping, cooling to room temperature, and obtaining the mixed chloroprene rubber.

And vulcanizing part of the mixed chloroprene rubber on a flat vulcanizing machine, taking out a sample, and testing the mechanical property of the sample, wherein the test result is shown in table 2.

TABLE 2 chloroprene rubber formulation Main Performance indices

Example 2

The male connector molding process comprises the following steps:

TABLE 3 Male connector device and tool

Serial number	Name (R)	Specification of	Use of
				01	Single core wire	Φ1.5mm	Details of
02	Butt terminal-male	/	Details of
				03	Copper shoulder pad	/	Details of
04	Positioning needle	Φ2.0*25mm	Details of
				05	Inlay	Φ8.0*2.8mm	Details of
06	CHEMLOK glue	205 and CH220	Binder
				07	Self-made rubber for connector	JTCR-4	Molded sample
08	Forming die 1 set	/	Molded sample
				09	Pressure sensor set	0-2000Kg	Monitoring glue injection pressure
10	Scissors, wire stripper, etc	/	Stripping the sheath of electric wire
				11	Welding gun and welding wire set	/	Welding wire and terminal
12	Jack	2T	Injection moulding of rubber material
				13	Flat vulcanizing agent	50T	Sample shaping
14	Forced air dryingBox	DHG-9035A	Preheating of mould and sizing material

1. Wire and stylet pretreatment

1.1 cutting out

Cutting the wires with the various colors and the outer diameter of 1.5mm into line segments with the length of 25cm for standby;

1.2 removing the wire cover

And (3) using a wire stripper to remove the outer skin of the cut electric wire and expose the inner copper core, wherein the length of the exposed part is 5mm.

1.3 welding wire and stylet

Welding the stripped electric wire and the needle core together by using a welding gun; the copper core needs to be inserted into the needle core to ensure the welding strength.

1.4 core surface treatment

And wiping the surface of the needle core by using alcohol to remove oil stains on the surface and the like. The cut insulating adhesive tape is used for covering the 8mm part of the top of the needle core, so that the part is prevented from being polluted in the subsequent gluing process.

And (3) coating the rest part of the needle core with a small amount of Chemlok 205 glue by using a fine brush, drying the wire and the needle core in an oven at 80 ℃ for 10min (or drying at room temperature for 30-60 min), coating finish paint Chemlok CH220 after the glue is solidified, and performing the same coating process.

And after the glue is dried, removing the adhesive tape coated on the top end of the needle core.

2. Pilot pin pretreatment

In the same way, the positioning pin surface is coated with the adhesives Chemlok 205 and CH220 glue, and the uncoated glue part length is 10mm.

3. Mold preheating

And (3) putting the forming die and the glue injection cylinder into an oven at 80 ℃, setting the temperature of a press to be 140 ℃, and preheating 1 hour in advance.

4. Mold assembly

After the procedures of welding the wire and the needle core, processing the surface of the needle core, preheating the mould and the like are finished, the operation of the step is carried out.

1) Four wires coated with adhesive and a stylet were taken and passed through the inlay hole.

2) And (3) placing the inlay and the electric wire into the socket main body, wherein the inlay is required to fall into a step phi 8 x 2.8mm in the socket.

3) And inserting each needle core and the positioning needle into corresponding holes of the mold core in sequence to ensure that the needle core completely enters the mold core.

4) And (3) putting the socket main body, the electric wire and the mold core into the bottom mold, and adjusting the angle of the mold core to ensure that the positioning pin is positioned right above the mold core.

5) The tail part of the electric wire is sleeved into the clamping device, and the tail part of the socket main body is sleeved into a central tube of the clamping device, so that the socket main body is ensured to be tightly matched with the clamping device.

6) And (5) closing the die, namely fastening the screws of the clamping device and fastening the fixed screws of the die.

5. Preheating of composite rubber material

The mixing preparation process refers to the relevant content in section 2.2, and the composite rubber material is made into a sheet with the thickness of 1-2mm in advance. After the die assembly is completed, 15-16g of composite rubber material film is weighed and placed in an oven at 80 ℃ for preheating for 3min.

6.1 injection device

And after the rubber material is preheated, taking out the rubber material and putting the rubber material into a preheated rubber injection cylinder. The equipment is annotated and is pressed device, from bottom to top do respectively: forming die, injecting glue jar, pressure sensor, jack. Note that material jar discharge gate should mould the hole of gluing on the standard mould.

6.2 injection moulding

And manually and slowly loading a jack, and injecting the rubber material into the mold. And observing the readings of the pressure sensor, and maintaining the glue injection pressure to be 10-12KN. And adopting a gradual injection mode, and loading the jack to pressurize when the pressure is lower than 10 KN. And when the reading descending rate of the sensor is less than 20N/s, the glue injection is finished.

6.3 disassembly

And (5) removing the pressure of the jack, taking down the jack and the sensor, and horizontally moving and detaching the glue injection cylinder from the upper surface of the die. Note that the glue injection cylinder and the mold should be prevented from being separated from each other, so that the glue in the glue injection runner of the mold is prevented from being carried out.

6. Vulcanization

And transferring the forming die to a preheated press, and vulcanizing and forming. The vulcanization process is 40min at 140 ℃.

7. Form removal

1) And after vulcanization, taking out the mold, and taking out the rubber material at the glue injection hole of the upper mold by using tools such as tweezers.

2) And sequentially disassembling the tightening sleeve screw and the die fixing screw.

3) Separating the upper die and the lower die, and carefully taking out the die core, the male plug product and the tightening sleeve.

4) And separating the tightening sleeve from the plug.

5) The core and the product are carefully separated, and if a tool such as pliers is needed, gauze is placed in the tool to prevent the surface of the product and the core from being damaged.

8. Sample surface treatment

And removing the flash on the surface of the product by using 1000-mesh sand paper, a wallpaper knife and other tools.

9. Tail encapsulation

1) Sample processing

And the adhesive tape is used for winding the surface of the sample, so that the sample is prevented from being polluted in the packaging process.

2) Sealant blending

Preheating the two components of the sealant in a 30 ℃ oven for 0.5h, weighing the sealant according to the proportion, and uniformly stirring. And putting the mixed rubber material into a vacuum oven, vacuumizing for 5min, and removing internal bubbles.

3) Package with a metal layer

And slowly injecting the sealant to the tail part of the common plug, slowly swinging the wire in the pouring process to accelerate the flow of the sealant, and stopping pouring when the sealant is slightly higher than the tail part of the common plug.

4) Curing

And (3) putting the poured plug into a 50 ℃ oven for curing for 6 hours, or curing at room temperature for more than 12 hours.

5) Surface treatment

The plug covering adhesive tape is stripped, and the surface of the plug is wiped by alcohol to remove stains.

Embodiment 3 female head molding process of connector:

watch 4 female head forming equipment and tool

1. Cable pretreatment

1.1 cutting out

The 4-core cable used was cut into 30cm length segments, noting that the ports were flush and perpendicular to the cable.

1.2 removing the Cable sheath

And (3) using a wire stripper to remove the outer skin of the cut cable and expose the inner wire core, wherein the distance between the wire stripping position and the cable port is 20mm. Separating the wire cores, and cutting off the filling material between the wire cores.

1.3 removing core cover

And stripping the envelope of each wire core by using a wire stripper to expose the internal copper wire, wherein the length of the exposed part is 3-5mm.

1.4 welding needle core

Welding 4 wire cores in the cable and the needle core together by using a welding gun; the copper core needs to be inserted into the needle core to ensure the welding strength. The outer surface of the core should not be built up by excess solder.

And after welding, checking whether the lengths of the 4 fiber cores are consistent, and if not, re-welding.

1.5 core needle surface treatment

1) And wiping the surface of the needle core by using alcohol to remove oil stains on the surface and the like.

2) And (3) dipping a small amount of Chemlok 205 glue by using a fine brush, coating the glue on the rest part of the needle core, drying the electric wire and the needle core in an oven at the temperature of 80 ℃ for 10min (or drying at room temperature for 30-60 min), coating a finish paint Chemlok CH220 after the glue is solidified, and coating the finish paint by using the same process.

3) After the Chemlok 205 and CH220 glue had dried, the tip was gently wiped with fine sandpaper to remove excess adhesive.

4) And (3) heating the cable in an oven at 150 ℃ for 20-30min to cure the adhesive on the surface of the needle core.

1.6 Cable surface treatment

1) And (3) carrying out sanding treatment on the part within 30mm of the rear end of the cable stripping position, and wiping the surface of the cable at the part by using 180-mesh abrasive paper.

2) Wiping the frosted cable surface with alcohol to remove stains.

3) And (3) uniformly coating the self-made binder NDW-2 on the needle core, the wire core and the surface of the cable subjected to the frosting treatment, repeatedly coating for 3-5 times, and drying at room temperature for 1 hour.

1.7 winding thread seal tape

Starting from a position of about 10-15mm after the adhesive part of the cable is coated, uniformly coating 3-4 layers of raw material belts on the surface of the cable, and preventing the cable from being damaged in the die pressing process.

2. Preheating of die and press

And (3) putting the forming die and the glue injection cylinder into an oven at 80 ℃, setting the temperature of a press to be 105 ℃, and preheating 1 hour in advance.

3. Mold assembly

After the winding of the raw material belt on the surface is finished, the operation of the step is carried out.

1) Preparing one composite rubber material film with the thickness less than 1mm in advance, cutting one rubber strip with the length of 100mm and the width of 5-8mm, and preheating for 2-3min at 80 ℃.

2) And sequentially inserting the four needle cores at the top end of the cable into the mold core, wherein no gap exists between the needle cores and the mold core positioning needles.

3) The preheated adhesive tape is uniformly wound on a cable pretreatment part, the adhesive tape is wound by one layer, the initial winding part is parallel and level, and the adhesive tape is prevented from being wound on an untreated part.

4) And (5) placing the cable and the mold core into the bottom mold to ensure that the positioning needle is positioned right above.

And (5) closing the die and fastening the corresponding screw.

5) And (4) placing the mold on a flat vulcanizing machine, applying working pressure, taking out the mold, and fastening corresponding screws again. The cable is prevented from slipping in the glue injection process.

4. Preheating of composite rubber material

The composite rubber material is made into a thin sheet with the thickness of 1-2mm in advance. After the mold assembly is completed, 15-16g of the composite rubber material film is weighed and placed in an oven at 80 ℃ for preheating for 3min.

5. Injection pressure

5.1 Assembly injection-compression device

And after the rubber material is preheated, taking out the rubber material and putting the rubber material into a preheated rubber injection cylinder. The equipment is annotated and is pressed device, from bottom to top do respectively: forming die, injecting glue jar, pressure sensor, jack. Note that material jar discharge gate should mould notes gluey hole on the standard mould.

5.2 injection of pressure

5.3 disassembly

And (4) removing the pressure of the jack, taking down the jack and the sensor, and horizontally moving and detaching the glue injection cylinder from the upper surface of the die. Note that the glue injection cylinder and the mold should be prevented from being separated from each other, so that the glue in the glue injection runner of the mold is prevented from being carried out.

6. Vulcanization

And transferring the forming die to a preheated press, and vulcanizing and forming. The press set temperature is 105 ℃, and the vulcanization time is 90min.

7. Form removal

2) And disassembling the die fixing screw.

3) Separating the upper and lower dies, and carefully taking out the die core and the product.

4) The core and the product are carefully separated, and if a tool such as pliers is needed, gauze is placed in the tool to prevent the surface of the product and the core from being damaged.

8. Sample surface treatment

Removing the raw material belt on the surface of the cable by using a wallpaper cutter; and removing the flash on the surface of the product by using 1000-mesh sand paper, a wallpaper knife and other tools.

Comparative example 1: the watertight connector was prepared using the formulation and process of examples 1-3, except that other grades of neoprene Baypren 112 were used; the results are shown in tables 7 and 8.

Comparative example 2: the watertight connector is prepared by adopting the formula and the process of the examples 1 to 3, and the difference is that ethylene propylene diene monomer is adopted;

as a result, the appearance of the sample was poor and there were many defects such as bubbling.

Comparative example 3: the watertight connector was prepared using the formulation and process of examples 1-3, except that butyl rubber was used; the results are shown in tables 7 and 8.

Comparative example 4: the watertight connector was prepared using the formulation and process of examples 1-3, except that 70 parts by weight of neoprene and 10 parts by weight of natural rubber were used; the results are shown in tables 7 and 8.

Comparative example 5: the watertight connector is prepared by adopting the formula and the process of the embodiment 1-3, and the difference is only that 32 parts by weight of tackifying master batch is adopted; the results are shown in tables 7 and 8.

Comparative example 6: the watertight connector is prepared by adopting the formula and the process of the examples 1 to 3, and the difference is only that 37 parts by weight of tackifying master batch is adopted;

the results were: the sample needle core and other matching parts are easy to enter rubber materials, the matching between the male head and the female head is poor, and the contact resistance is high.

Comparative example 7: the watertight connector is prepared by adopting the formula and the process of the embodiments 1 to 3, and the difference is only that modified talcum powder 33 is adopted; the results are shown in tables 7 and 8.

Comparative example 8: the watertight connector was prepared using the formulation and process of examples 1-3, except that modified talc powder 37 was used;

the results were: the flowability of the rubber compound is poor, and the rubber part of the sample has deletion.

Comparative example 9: the watertight connector was prepared using the formulation and process of examples 1-3, except that 0.8 parts by weight of insoluble sulfur; the results are shown in tables 7 and 8.

Comparative example 10: the watertight connector was prepared using the formulation and process of examples 1-3, except that 1.2 parts by weight of insoluble sulphur was used;

the results were: the product is easy to tear in the process of removing the mould, and the yield is low.

Comparative example 11: the watertight connector was prepared using the formulation and process of examples 1-3, except that no processing aid was added;

the results were: the mold sticking phenomenon exists after the product is vulcanized, and the outer surface of part of the product is torn.

Comparative example 12: the watertight connector was prepared using the formulations and processes of examples 1-3, except that no accelerator was added; the results are shown in tables 7 and 8.

Comparative example 13: the watertight connector is prepared by adopting the formula and the process of the examples 1 to 3, and the difference is that the accelerant is other types, specifically the accelerant CZ; the results are shown in tables 7 and 8.

Comparative example 14: the watertight connector is prepared by adopting the formula and the process of the embodiment 1-3, and the pressure of glue injection is 9KN;

as a result, the rubber portion of the sample was not complete, and defects such as starved feeding and dishing were observed.

Comparative example 15: the watertight connector is prepared by adopting the formula and the process of the embodiment 1-3, and the pressure of glue injection is 13KN;

as a result, a large amount of sizing material enters the female needle core, the female needle core cannot be used, and the product yield is low.

Comparative example 16: the preheating of the composite rubber material comprises the following steps: preparing the composite rubber material into a film with the thickness of 3mm, weighing 15-16g of the film after the die and the accessory are assembled, putting the film into a drying oven at 90 ℃, and preheating for 3min.

As a result, the material loss is high in the glue injection process, and the product is not prepared successfully.

Comparative example 17: the preheating of the composite rubber material comprises the following steps: preparing the composite rubber material into a film with the thickness of 2mm, weighing 15-16g of the film after the die and the accessory are assembled, putting the film into an oven at 80 ℃, and preheating for 5min.

The result is that the preheating is excessive, the material before injecting glue has slight cross-linking, the fluidity is reduced, and the surface of the product has more glue injection marks and is not smooth.

Experimental example 1

The physical properties of the watertight connectors manufactured according to the methods of examples 1 to 3 are specified in Table 5.

TABLE 5 connector physical Property parameters

Wherein, the rebound resilience after pressurization refers to the rebound resilience after 5 minutes after the pressure is maintained for 24 hours under the water depth of 6000 meters.

The electrical parameters of the rubber pressure-resistant watertight connector are detailed in table 6.

TABLE 6 electric performance parameters of the rubber pressure-resistant watertight connector

The rubber pressure-resistant watertight connector prepared by the method has smooth and flat outer surfaces of a male head (socket) and a female head (plug) of the connector, and has no cracks, bubbles, peeling and damage. The rubber, the copper shell and the conductive needle core are not dropped off, no excess adhesive is used, and no glue is left on each bonding surface. The rubber pressure-resistant watertight connector can be operated in a deep sea environment, maintains good sealing performance and good mechanical performance, particularly water pressure resistance, meets the current deep sea coverage, and meets the stable electric transmission use requirement.

The performance parameters of the comparative examples are shown in tables 7 and 8:

TABLE 7

"not tested" means that there is no detection meaning (the first several indexes are not qualified, and the plugging and unplugging times test is time-consuming, labor-consuming, and unnecessary), so that the detection is not performed.

TABLE 8

	Insulation resistance (M omega)	Contact resistance (omega)
			Index (I)	≥500	≤0.01
Comparative example 1	600	0.005
			Comparative example 3	600	0.005
Comparative example 4	900	0.004
			Comparative example 5	1700	0.003
Comparative example 7	1700	0.003
			Comparative example 9	1750	0.003
Comparative example 12	1500	0.005
			Comparative example 13	600	0.007

Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims

1. A method for manufacturing a watertight connector, characterized by comprising at least the following steps:

s1, preparing a composite rubber material; the raw materials of the composite rubber material comprise 79.5 to 80.5 weight parts of chloroprene rubber, 34.5 to 35.5 weight parts of tackifying master batch, 0.95 to 1.05 weight parts of insoluble sulfur, 4.7 to 5.2 weight parts of zinc oxide, 34 to 36 weight parts of silane coupling agent modified talcum powder, 3 to 5 weight parts of magnesium oxide, 0.5 to 1.5 weight parts of anti-aging agent, 0.5 to 1.5 weight parts of stearic acid, 1.5 to 2.5 weight parts of accelerator and 0.45 to 0.55 weight part of carbon black N330; the chloroprene rubber is selected from chloroprene rubber Baypren711; the accelerant is selected from N, N' -dibutyl thiourea; the anti-aging agent is 4020NA;

the tackifying master batch comprises 20 parts by weight of chloroprene rubber, 8-12 parts by weight of terpene resin and 5 parts by weight of silane coupling agent modified talcum powder;

banburying and mixing are carried out on the composite rubber material to obtain mixed rubber;

the pressure of the glue injection is 10-12KN.

2. The preparation method according to claim 1, wherein the raw materials of the composite rubber material are as follows: 80 parts of chloroprene rubber, 35 parts of tackifying master batch, 35 parts of silane coupling agent modified talcum powder, 1 part of insoluble sulfur, 5 parts of zinc oxide, 4 parts of magnesium oxide, 1 part of anti-aging agent, 1 part of stearic acid, 2 parts of accelerator and 0.5 part of carbon black N330;

the tackifying master batch comprises the following components: 20 parts of chloroprene rubber, 10 parts of terpene resin and 5 parts of silane coupling agent modified talcum powder.

3. The method for preparing the watertight connector according to claim 1, wherein the watertight connector comprises a male head and a female head, the fitting of the male head comprises a needle core, an electric wire, a positioning needle, a copper shell and a rubber wrap, and the fitting of the female head comprises an electric conduction jack, a cable and a rubber wrap;

the fittings of the pretreatment watertight connector comprise electric wires and a stylet pretreatment and a positioning needle pretreatment;

4. The method of claim 3, wherein the wire and core pretreatment comprises: cutting an electric wire, removing a cover of the electric wire, welding the electric wire and the stylet, and carrying out surface treatment on the stylet;

5. The method of claim 3, wherein the mold preheating comprises: and (3) putting the male head die, the female head die and the glue injection cylinder into an oven at 80 ℃, setting the temperature of a press to be 140 ℃, and preheating 1 hour in advance.

6. The method of claim 1, wherein the pre-heating of the composite rubber material comprises: preparing the composite rubber material into a film with the thickness of 1-2mm, weighing 15-16g of the film after the die and the accessory are assembled, putting the film into a baking oven with the temperature of 75-85 ℃, and preheating for 2.5-3.0min.

7. The preparation method according to claim 1, wherein in the glue injection process, when the reading drop rate of the pressure sensor is less than 20N/s, the glue injection is completed; in the glue injection process, a gradual injection and pressing mode is adopted; the pressurizing speed is 10KN/min, and when the pressure is lower than 10KN, the jack is loaded for pressurizing; the vulcanization condition is that the treatment is carried out for 40min at 140 ℃; the post-treatment comprises demolding and sample surface treatment.

8. A watertight connector manufactured by the manufacturing method according to any one of claims 1 to 7.

9. The composite rubber material is characterized by being prepared from the following raw materials: 80 parts of chloroprene rubber, 35 parts of tackifying master batch, 34-36 parts of silane coupling agent modified talcum powder, 1 part of insoluble sulfur, 5 parts of zinc oxide, 3-5 parts of magnesium oxide, 0.5-1.5 parts of anti-aging agent, 0.5-1.5 parts of stearic acid, 1.5-2.5 parts of accelerator and 0.5 part of carbon black N330; the tackifying master batch comprises 20 parts by weight of chloroprene rubber, 8-12 parts by weight of terpene resin and 5 parts by weight of silane coupling agent modified talcum powder; the chloroprene rubber is selected from chloroprene rubber Baypren711; the accelerant is selected from N, N' -dibutyl thiourea; the anti-aging agent is 4020NA.

10. The compounded rubber material according to claim 9, wherein the compounded rubber material is prepared from the following raw materials: 80 parts of chloroprene rubber, 35 parts of tackifying master batch, 35 parts of silane coupling agent modified talcum powder, 1 part of insoluble sulfur, 5 parts of zinc oxide, 4 parts of magnesium oxide, 1 part of anti-aging agent, 1 part of stearic acid, 2 parts of accelerator and 0.5 part of carbon black N330; the tackifying master batch comprises the following components: 20 parts of chloroprene rubber, 10 parts of terpene resin and 5 parts of silane coupling agent modified talcum powder.

11. Use of a composite rubber material according to any one of claims 9 to 10 for the preparation of watertight fittings.

12. The use according to claim 11, wherein the pressure during glue injection is 10-12KN when the composite rubber material is used for preparing a watertight device.