CN113403126B - Environment-friendly flame-retardant water-blocking paste for communication optical cable and preparation method thereof - Google Patents

Environment-friendly flame-retardant water-blocking paste for communication optical cable and preparation method thereof Download PDF

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CN113403126B
CN113403126B CN202110635868.9A CN202110635868A CN113403126B CN 113403126 B CN113403126 B CN 113403126B CN 202110635868 A CN202110635868 A CN 202110635868A CN 113403126 B CN113403126 B CN 113403126B
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retardant
environment
flame
water
flame retardant
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CN113403126A (en
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乔传威
郑金周
刘仲毅
王静礼
梁浩勇
李卫东
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Zhengzhou Oupushi Technology Co ltd
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Abstract

The application relates to the technical field of communication optical cables, in particular to an environment-friendly flame-retardant water-blocking paste for a communication optical cable and a preparation method thereof. The preparation raw materials comprise the following components in parts by weight: 1 to 6 parts of inorganic thickening agent, 8 to 20 parts of gelatinizing agent, 30 to 70 parts of base oil, 12 to 30 parts of flame retardant and 3 to 12 parts of other auxiliary agents; the inorganic thickening agent is modified sodium bentonite. The environment-friendly flame-retardant waterproof paste adopts a proper amount of quaternary ammonium salt modified sodium bentonite in raw materials, and adjusts components and proportion of base oil, so that the high-low temperature applicability of the environment-friendly flame-retardant waterproof paste is remarkably improved, the environment-friendly flame-retardant waterproof paste has a higher dropping point, and the environment-friendly flame-retardant waterproof paste has lower cone penetration degree at normal temperature and 40 ℃ below zero. Meanwhile, the hydrogenated styrene-isoprene copolymer and a proper amount of modified silica gel are adopted as the gelling agent, so that the water blocking performance of the flame-retardant water blocking paste is improved to a great extent, and especially, the water blocking performance of the flame-retardant water blocking paste is further improved by compounding a proper amount of ethylene oxide/propylene oxide block copolyether, neutral barium dinonylnaphthalene sulfonate and other components.

Description

Environment-friendly flame-retardant water-blocking paste for communication optical cable and preparation method thereof
Technical Field
The application relates to the technical field of communication optical cables, in particular to an environment-friendly flame-retardant water-blocking paste for a communication optical cable and a preparation method thereof.
Background
With the rapid development of the communication industry in China, the use amount of optical cables is increasing. In the use process, the change of the surrounding environment of the optical cable can cause the air pressure difference between the inside and the outside of the sheath tube to cause the non-directional diffusion of moisture from the outside of the optical cable to the inside, and finally, the inside of the optical cable can generate undesirable high humidity, so that the transmission performance of the optical cable can be greatly damaged; at the same time, water may enter the optical cable due to damage, and flow toward the hinge closure in the longitudinal direction, resulting in serious performance degradation. Therefore, there is a need for an optical cable filling paste having excellent water blocking properties.
Not only moisture and humidity, the optical cable also faces hydrogen loss generated in a hydrogen evolution environment, and when the optical cable is further subjected to stress, corrosion and hydrogen loss, the transmission performance of optical cable information can be greatly reduced. The most fatal phenomenon is that under extremely severe high-temperature weather conditions, the spontaneous combustion phenomenon of an insulating wire core material is caused by overlarge current among optical cable conductors caused by instantaneous overload and overhigh voltage, so that the information transmission performance can be completely lost, and serious consequences are caused to national construction and social life. Therefore, there is a need for an optical cable filling paste having excellent flame retardant properties. Meanwhile, under the condition of spontaneous combustion, the optical cable filling paste is easy to run off at high temperature and drop to the field ground environment to cause land pollution, so that the invention pays attention to environmental protection performance and has excellent biodegradability.
In the current optical cable filling ointment, the common cable ointment is mostly adopted to prevent the optical cable from water seepage and moisture, only has the water blocking effect, has no relevant manufacturer or relevant product in the aspects of flame retardant property and environmental protection property, and simultaneously combines the three properties.
Disclosure of Invention
Aiming at the technical problems, the first aspect of the invention provides an environment-friendly flame-retardant water-blocking paste, which comprises the following raw materials in parts by weight:
1 to 6 portions of inorganic thickening agent
Gelling agent 8-20
Base oil 30-70
12 to 30 portions of flame retardant
3-12 of other auxiliary agents;
the inorganic thickening agent is modified sodium bentonite.
As a preferable technical scheme of the invention, the modified sodium bentonite is quaternary ammonium salt modified sodium bentonite.
As a preferred embodiment of the present invention, the base oil comprises trimellitate and pentaerythritol ester; preferably, the mass ratio of the trimellitate to the pentaerythritol ester is (25-35): (15-24).
As a preferable technical scheme of the invention, the kinematic viscosity of the pentaerythritol ester at 100 ℃ is 27-30 mm 2 /s。
As a preferred embodiment of the present invention, the gelling agent comprises a hydrogenated styrene-isoprene copolymer; preferably, the content of the hydrogenated styrene-isoprene copolymer accounts for 6-12 wt% of the total amount of the raw materials for preparing the environment-friendly flame-retardant water-blocking paste.
As a preferred embodiment of the invention, the further auxiliary comprises an ethylene oxide/propylene oxide block copolyether.
As a preferable technical scheme of the invention, the flame retardant is a mixture of organic phosphate liquid flame retardant and phosphorus-nitrogen flame retardant powder flame retardant.
As a preferred embodiment of the present invention, the other auxiliary agent comprises a smoke suppressor; the smoke suppressor consists of ferrocene, zinc molybdate, melamine hydroxy stannate and zinc hydroxystannate; preferably, the weight ratio of ferrocene, zinc molybdate, melamine hydroxystannate and zinc hydroxystannate is 1:2:1:1.
The second aspect of the invention provides a preparation method of the environment-friendly flame-retardant water-blocking paste, which comprises the following steps:
(1) According to the proportion, the base oil is pumped into a fat making kettle, the temperature is raised to 50-70 ℃, the gelatinizing agent is added, the stirring and the temperature are continuously raised to 160-180 ℃, and the base oil is transferred into a blending kettle;
(2) Cooling the raw materials of the blending kettle to 130-140 ℃, adding an inorganic thickening agent, and circulating a shearing machine for 2-4 hours, wherein the shearing pressure is regulated to 1.0-1.2 MPa;
(3) Then cooling to 70-80 ℃, adding other auxiliary agents, continuously circularly shearing for 0.5-2 hours, reducing the shearing pressure to zero, adding the rest raw materials, continuously stirring and circularly recycling for 1 hour, and finally obtaining the finished product.
The third aspect of the invention provides application of the environment-friendly flame-retardant water-blocking paste, which is applied to the technical field of communication optical cables.
The beneficial effects are that: the environment-friendly flame-retardant waterproof paste adopts a proper amount of quaternary ammonium salt modified sodium bentonite in raw materials, and adjusts components and proportion of base oil, so that the high-low temperature applicability of the environment-friendly flame-retardant waterproof paste is remarkably improved, the environment-friendly flame-retardant waterproof paste has a higher dropping point, and the environment-friendly flame-retardant waterproof paste has lower cone penetration degree at normal temperature and 40 ℃ below zero. Meanwhile, the hydrogenated styrene-isoprene copolymer and a proper amount of modified silica gel are adopted as the gelling agent, so that the water blocking performance of the flame-retardant water blocking paste is improved to a great extent, and especially, the water blocking performance of the flame-retardant water blocking paste is further improved by compounding a proper amount of ethylene oxide/propylene oxide block copolyether, neutral barium dinonylnaphthalene sulfonate and other components. In addition, the application adopts the mixture of the organic phosphate liquid flame retardant and the phosphorus-nitrogen flame retardant powder, and simultaneously uses the smoke suppressor composed of ferrocene, zinc molybdate, melamine hydroxy stannate and zinc hydroxy stannate in a compounding way, and the mutual synergistic effect is utilized to obviously improve the flame retardant property of the water-blocking paste, so that the water-blocking paste has more excellent comprehensive performance.
Drawings
Fig. 1 is a physical diagram of an environment-friendly flame-retardant water-blocking paste product of the application.
Fig. 2 is a physical diagram of an environment-friendly flame-retardant water-blocking paste product of the present application.
Detailed Description
The contents of the present invention can be more easily understood by referring to the following detailed description of preferred embodiments of the present invention and examples included. 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. In case of conflict, the present specification, definitions, will control.
The terms "comprising," "including," "having," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
When an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. Furthermore, the indefinite articles "a" and "an" preceding an element or component of the invention are not limited to the requirements of the number of elements or components (i.e. the number of occurrences). Thus, the use of "a" or "an" should be interpreted as including one or at least one, and the singular reference of an element or component also includes the plural reference unless the amount is obvious to the singular reference.
The kinematic viscosity is the ratio of hydrodynamic viscosity to the density ρ of the fluid at the same temperature, and is a physical quantity representing the viscosity of the components, and is obtained by testing in a conventional manner in the art. The viscosity index as used herein refers to the degree to which the viscosity of all fluids changes with temperature. The higher the viscosity index, the less the fluid viscosity is affected by temperature, the less the viscosity is sensitive to temperature, as tested in conventional fashion.
The first aspect of the invention provides an environment-friendly flame-retardant water-blocking paste, which comprises the following raw materials in parts by weight:
1 to 6 portions of inorganic thickening agent
Gelling agent 8-20
Base oil 30-70
12 to 30 portions of flame retardant
3-12 of other auxiliary agents;
the inorganic thickening agent is modified sodium bentonite.
In some embodiments, the modified sodium bentonite is a quaternary ammonium salt modified sodium bentonite. The Zhejiang Hongyu New Material Co., ltd, code HY738 can be selected.
In some embodiments, the base oil comprises trimellitate and pentaerythritol esters;
pentaerythritol esters described in the present application areSaturated polyol ester POE formed by the reaction of pentaerythritol and high and low carbon fatty acid. In some embodiments, the pentaerythritol esters have a Viscosity Index (VI) of 120 to 125; further preferably, the pentaerythritol ester has a kinematic viscosity of 288-352 mm at 40 DEG C 2 S (preferably 320 mm) 2 S); it is further preferred that the kinematic viscosity at 100℃is 27 to 30mm 2 S (preferably 29 mm) 2 S); preferably, the mass ratio of the trimellitate to the pentaerythritol ester is (25-35): (15-24). The code POE320 of Yingkou star fire chemical industry Co., ltd.
The trimellitate is saturated polyol ester formed by reacting trimellitic acid (namely 1,2, 4-benzene tricarboxylic acid) with high-carbon and low-carbon fatty acid, and can be identified by the code number S150 of Yingkou star fire chemical industry Co.
The applicant finds that when a proper amount of quaternary ammonium salt modified sodium bentonite is adopted in the environment-friendly flame-retardant water-blocking paste raw material, and after the base oil components and the proportion are adjusted, the high-low temperature applicability of the environment-friendly flame-retardant water-blocking paste can be obviously improved, so that the environment-friendly flame-retardant water-blocking paste has a higher dropping point and has lower cone penetration under the environment of normal temperature and minus 40 ℃. Especially when trimellitate and pentaerythritol ester are used as base oil, the quaternary ammonium salt modified sodium bentonite is used in an amount of 3-4wt% to improve the performance remarkably. The applicant speculates that the quaternary ammonium salt modified sodium bentonite has slow response speed to high temperature stimulus due to the bentonite structure contained in the structure, and is relatively stable at high temperature. Meanwhile, the bentonite is uniformly dispersed in the system by the quaternary ammonium salt long-chain structure in the structure, the components in the system are entangled by the long polymer chain segment, and external stimulus is consumed at low temperature in an elastic deformation mode and the like, so that the stability of the flame-retardant water-blocking paste at low temperature is improved. Particularly, when the system comprises trimellitic acid ester and pentaerythritol ester in a specific proportion as base oil, a branched chain structure in the base oil structure can be randomly inserted into the system, and the branched chain structure and a quaternary ammonium salt structure in a modified sodium bentonite structure are together used for firmly stabilizing the rest components in the system in a formed space network, and external stimulus is consumed through the stable network, so that the high-low temperature stability performance of the flame-retardant water-blocking paste is effectively improved. In addition, through the stable network structure, the microstructure density of the flame-retardant water-blocking paste is improved to a great extent, and the water-blocking performance of the flame-retardant water-blocking paste is remarkably improved.
In some embodiments, the gellant comprises a hydrogenated styrene-isoprene copolymer; preferably, the content of the hydrogenated styrene-isoprene copolymer accounts for 6-12 wt% of the total amount of the raw materials for preparing the environment-friendly flame-retardant water-blocking paste. The hydrogenated styrene-isoprene copolymer can form a gel state in a system, is beneficial to improving the dropping point of the hydrogenated styrene-isoprene copolymer and controlling oil distribution, and can be selected from the product of China petrochemical industry Co., ltd.
Further preferably, the gelling agent further comprises a modified silica gel; the addition of a proper amount of modified silica gel in the application is favorable for improving the insulating property and the damping property of the flame-retardant waterproof paste, and the flame-retardant property of the flame-retardant waterproof paste can be improved to a great extent. A product with a code JW-E600 of Shenzhen gold Wang Keji Co., ltd.
In some embodiments, the other adjuvant comprises an ethylene oxide/propylene oxide block copolyether. The ethylene oxide/propylene oxide block copolyether structure contains a hydrophilic ether chain segment, also contains a hydrophobic aliphatic alkyl chain, has surface tension at the bottom of the cross, is favorable for destroying micelles formed by emulsification in a system, prevents water vapor from penetrating into the paste, has super-strong hydrolytic resistance, and can be selected from Qingdao Sofu wetting chemical technology Co., ltd.
The applicant found that when hydrogenated styrene-isoprene copolymer and a proper amount of modified silica gel are used as the gelling agent, the water blocking performance of the flame-retardant water blocking paste is improved to a great extent, and particularly when a proper amount of ethylene oxide/propylene oxide block copolyether is added into the system, the water blocking performance is improved remarkably. The hydrogenated styrene-isoprene copolymer structure comprises a rigid benzene ring structure and a flexible aliphatic alkyl chain, and is easy to form a gel state when being added into the system, so that other components in the system are stabilized, the dropping point of the water-blocking paste is improved, and the phenomenon of oil separation under high temperature and other environments is avoided. Meanwhile, as some small molecular ester base oil, modified sodium bentonite and other components in the system have certain hydrophilicity, water in the environment can permeate into the flame-retardant water-blocking paste and form a water-in-oil emulsion structure, so that the water blocking performance of the flame-retardant water-blocking paste is hindered, and the addition of the ethylene oxide/propylene oxide block copolyether is favorable for damaging water-in-oil micelles formed in the system, avoiding further permeation of water molecules and even extruding water molecules out of the system, so that the water blocking performance of the flame-retardant water-blocking paste is favorable for improving. In addition, the applicant found that when the system contains neutral barium dinonylnaphthalene sulfonate as an antirust agent, the water blocking effect is better.
In some embodiments, the flame retardant is a mixture of an organic phosphate liquid flame retardant and a phosphorus-nitrogen flame retardant powder flame retardant. The organic phosphate flame retardant is liquid, has high phosphorus content, and can be selected from Nanjing Sier chemical production, and the code number is HR-105. The phosphorus-nitrogen flame retardant powder flame retardant is in a powder shape, has high phosphorus content, good heat stability, high hydrophobicity, hydrolysis resistance, high temperature resistance and no migration, and good carbon forming property, and can be selected from Nanjing Sier chemical production, code number HR-202 products.
In some embodiments, the other adjunct comprises a smoke suppressant; the smoke suppressor consists of ferrocene, zinc molybdate, melamine hydroxy stannate and zinc hydroxystannate; preferably, the weight ratio of ferrocene, zinc molybdate, melamine hydroxystannate and zinc hydroxystannate is 1:2:1:1.
The flame retardant in the application is preferably a mixture of an organic phosphate flame retardant and phosphorus-nitrogen flame retardant powder, and the flame retardant performance of the flame retardant and water-blocking paste is found to be remarkably improved. On the one hand, the organic phosphate flame retardant has higher phosphorus content, and the heated degradation product of the organic phosphate flame retardant is utilized to promote the surface of the flame-retardant substrate to be rapidly dehydrated and carbonized, so that the carbonized layer is formed because the simple substance carbon does not carry out evaporation combustion and decomposition combustion for generating flame. Meanwhile, because the phosphorus-nitrogen flame retardant powder contains the phosphine and the nitrogen-containing components in the structure, the phosphorus-nitrogen flame retardant powder is prevented from further burning in a condensed phase and a gas phase, and thus the synergistic effect is achieved, and a better flame retardant effect is realized. On the other hand, as the organic phosphate flame retardant is not liquid flame retardant, the phosphorus-nitrogen flame retardant powder is powdery flame retardant, and the components can be more uniformly dispersed when the raw materials of the flame-retardant water-blocking paste are prepared by blending, so that better uniformity and higher bulk density are realized, and the phosphorus-nitrogen flame retardant powder has better stability at high temperature and cannot migrate due to factors such as high temperature, so that the flame retardant effect of the phosphorus-nitrogen flame retardant powder is further synergistically improved. In addition, the smoke suppressor in the present application is composed of ferrocene, zinc molybdate, melamine hydroxystannate, zinc hydroxystannate, and these components can adsorb smoke particles generated by combustion when combustion occurs, and avoid flying. At the same time, the adsorbed smoke dust particle components are helpful for promoting the dehydration carbonization speed of the surface of the water-blocking paste, and can cooperate with the organic phosphate flame retardant and the phosphorus-nitrogen flame retardant powder to further thicken and dehydrate the thickness of the carbon layer, thereby further improving the flame retardant property of the water-blocking paste.
Other adjuvants in this application may be dispersion aids for aiding the gelling agent, base oil, flame retardant, smoke suppressant, etc. components in a uniform dispersion, including but not limited to propylene carbonate.
The other auxiliary agents in the application can also be modified nano white carbon black, preferably the modified nano white carbon black is prepared by adopting a weather method, the preferred particle size is 10-30 nm, and the oil separation of the system is restrained by utilizing a large number of micropore structures of the modified nano white carbon black, and the modified nano white carbon black can be selected from the products of the Weifang scintillant nano material Co, code HS-9280.
Other auxiliary agents in the present application may also be antioxidants, including but not limited to 2, 6-di-T-butyl-p-cresol (T501), etc., which can absorb free radicals generated by decomposition in the system and thereby avoid damage to the microstructure of the paste from these free radicals.
Other adjuvants in the present application may also be rust inhibitors, including but not limited to barium neutral dinonylnaphthalene sulfonate, having certain anti-salt spray properties, rust inhibitive properties and anti-emulsifying properties.
The applicant finds that the flame retardant property and the water blocking property of the flame retardant water blocking paste can be improved to a great extent after a proper amount of modified nano white carbon black and propylene carbonate are added into the system. Wherein propylene carbonate can improve the full dispersion among the raw materials in the system, so that the flame retardant components and the components which are beneficial to water blocking in the system can be distributed more uniformly and compactly. On the one hand, the modified nano white carbon black utilizes a large amount of void structures on the structure, so that the entry and migration of water vapor are avoided, and the water blocking performance of the modified nano white carbon black is improved. Of course, the multi-void structure is also helpful for absorbing the micromolecular ester base oil in the system, and the unstable phenomenon of oil seepage, oil separation and the like under the environment of high temperature and the like is avoided. On the other hand, a coacervate phase is formed during combustion, heat is quickly transferred, and the effects of heat conduction and temperature reduction are achieved, so that the flame retardance and smoke abatement effects are further improved.
The second aspect of the invention provides a preparation method of the environment-friendly flame-retardant water-blocking paste, which comprises the following steps:
(1) According to the proportion, the base oil is pumped into a fat making kettle, the temperature is raised to 50-70 ℃, the gelatinizing agent is added, the stirring and the temperature are continuously raised to 160-180 ℃, and the base oil is transferred into a blending kettle;
(2) Cooling the raw materials of the blending kettle to 130-140 ℃, adding an inorganic thickening agent, and circulating a shearing machine for 2-4 hours, wherein the shearing pressure is regulated to 1.0-1.2 MPa;
(3) Then cooling to 70-80 ℃, adding other auxiliary agents, continuously circularly shearing for 0.5-2 hours, reducing the shearing pressure to zero, adding the rest raw materials, continuously stirring and circularly recycling for 1 hour, and finally obtaining the finished product.
Further, the preparation method of the environment-friendly flame-retardant water-blocking paste comprises the following steps:
(1) Mixing base oil of trimellitate and pentaerythritol ester according to a proportion, and pumping the base oil into a fat manufacturing kettle; heating to 60 ℃, adding the hydrogenated styrene-isoprene copolymer, continuously stirring and heating to 170 ℃, and transferring into a blending kettle.
(2) Adding modified silica gel into the blending kettle, and stirring for 30 minutes; and (3) opening water cooling, cooling to 130-140 ℃, closing the water cooling, adding the modified sodium bentonite and the propylene carbonate, opening a circulating shearing machine after the modified sodium bentonite and the propylene carbonate are completely dispersed, and shearing the materials for 3 hours under the shearing pressure of 1.0-1.2 MPa.
(3) And (3) opening a water-cooling device, cooling to 70-80 ℃, sequentially adding an antioxidant, an antirust agent and a demulsifier, continuously circularly shearing for 1 hour, and then reducing the shearing pressure to zero.
(4) Sequentially adding modified nano white carbon black, an organic phosphate flame retardant, a phosphorus-nitrogen flame retardant powder mixture and a smoke suppressor, and continuously circulating for 1 hour; homogenizing, degassing, and transferring into a finished product tank.
The third aspect of the invention provides application of the environment-friendly flame-retardant water-blocking paste, which is applied to the technical field of communication optical cables.
The present invention will be specifically described below by way of examples. It is noted herein that the following examples are given by way of further illustration of the present invention and are not to be construed as limiting the scope of the present invention, since numerous insubstantial modifications and adaptations of the invention to those skilled in the art in light of the foregoing disclosure will still fall within the scope of the present invention wherein the demulsifier is an ethylene oxide/propylene oxide block copolyether; the trimellitates described in the following examples and comparative examples were selected from the commercial products of the chemical industry, inc., with the code number S150.
Example 1
The embodiment provides an environment-friendly flame-retardant water-blocking paste, which comprises the following components in the formula table 1:
TABLE 1
Component \ Content of
Modified sodium bentonite 3.5
Modified silica gel 4
Trimellitic acid ester 33.2
Pentaerythritol esters 24
Hydrogenated styrene-isoprene copolymer 9
Propylene carbonate 1.1
Modified nano white carbon black 2
2, 6-Di-tert-butyl-p-cresol 0.8
Neutral barium dinonyl naphthalene sulfonate 0.7
Ethylene oxide/propylene oxide block copolyethers 0.2
Organic phosphate flame retardant 16
Phosphorus-nitrogen flame retardant powder mixture 3
Smoke eliminator 2.5
Wherein, the modified sodium bentonite adopts Zhejiang Hongyu new material Co., ltd, and the product with the code HY 738; the modified silica gel adopts Shenzhen Jin Wang Keji Co., ltd, code JW-E600 product; pentaerythritol ester is a POE320 product of Yingkou star fire chemical industry Co., ltd; the hydrogenated styrene-isoprene copolymer adopts the product with the code SEP YH-4010 of the petrochemical company, basil, china petrochemical Co., ltd; modified nano white carbon black adopts a product of Weifang constant scintillation nano material limited company, code HS-9280; the ethylene oxide/propylene oxide block copolyether adopts a product with the code DL-32 of Qingdao Sofu wetting chemical engineering Co., ltd; the organic phosphate flame retardant adopts Nanjing Sier chemical production, and the product is named HR-105; the phosphorus-nitrogen flame retardant powder mixture is produced by Nanjing Sier chemical industry, and the product is named HR-202; the smoke suppressor is ferrocene: zinc molybdate: melamine hydroxystannate and zinc hydroxystannate in the mass ratio of 1:2:1:1.
The preparation method of the environment-friendly flame-retardant water-blocking paste comprises the following steps:
(1) Mixing base oil of trimellitate and pentaerythritol ester according to a proportion, and pumping the base oil into a fat manufacturing kettle; heating to 60 ℃, adding the hydrogenated styrene-isoprene copolymer, continuously stirring and heating to 170 ℃, and transferring into a blending kettle.
(2) Adding modified silica gel into the blending kettle, and stirring for 30 minutes; and (3) opening water cooling, cooling to 135 ℃, closing the water cooling, adding the modified sodium bentonite and the propylene carbonate, opening a circulating shearing machine, adjusting the shearing pressure to 1.1MPa, and shearing for 3 hours after the modified sodium bentonite and the propylene carbonate are completely dispersed.
(3) And (3) opening a water-cooling device, cooling to 75 ℃, sequentially adding an antioxidant, an antirust agent and a demulsifier, continuously circularly shearing for 1 hour, and then reducing the shearing pressure to zero.
(4) Sequentially adding modified nano white carbon black, an organic phosphate flame retardant, a phosphorus-nitrogen flame retardant powder mixture and a smoke suppressor, and continuously circulating for 1 hour; homogenizing, degassing, and transferring into a finished product tank.
Example 2
The embodiment provides an environment-friendly flame-retardant water-blocking paste, which comprises the following components in the formula table 2:
TABLE 2
Figure BDA0003105678830000091
Figure BDA0003105678830000101
Wherein, the modified sodium bentonite adopts Zhejiang Hongyu new material Co., ltd, and the product with the code HY 738; the modified silica gel adopts Shenzhen Jin Wang Keji Co., ltd, code JW-E600 product; pentaerythritol ester is a POE320 product of Yingkou star fire chemical industry Co., ltd; the hydrogenated styrene-isoprene copolymer adopts the product with the code SEP YH-4010 of the petrochemical company, basil, china petrochemical Co., ltd; modified nano white carbon black adopts a product of Weifang constant scintillation nano material limited company, code HS-9280; the ethylene oxide/propylene oxide block copolyether adopts a product with the code DL-32 of Qingdao Sofu wetting chemical engineering Co., ltd; the organic phosphate flame retardant adopts Nanjing Sier chemical production, and the product is named HR-105; the phosphorus-nitrogen flame retardant powder mixture is produced by Nanjing Sier chemical industry, and the product is named HR-202; the smoke suppressor is ferrocene: zinc molybdate: melamine hydroxystannate and zinc hydroxystannate in the mass ratio of 1:2:1:1.
The preparation method of the environment-friendly flame-retardant water-blocking paste comprises the following steps:
(1) Mixing base oil of trimellitate and pentaerythritol ester according to a proportion, and pumping the base oil into a fat manufacturing kettle; heating to 60 ℃, adding the hydrogenated styrene-isoprene copolymer, continuously stirring and heating to 170 ℃, and transferring into a blending kettle.
(2) Adding modified silica gel into the blending kettle, and stirring for 30 minutes; and (3) opening water cooling, cooling to 135 ℃, closing the water cooling, adding the modified sodium bentonite and the propylene carbonate, opening a circulating shearing machine, adjusting the shearing pressure to 1.1MPa, and shearing for 3 hours after the modified sodium bentonite and the propylene carbonate are completely dispersed.
(3) And (3) opening a water-cooling device, cooling to 75 ℃, sequentially adding an antioxidant, an antirust agent and a demulsifier, continuously circularly shearing for 1 hour, and then reducing the shearing pressure to zero.
(4) Sequentially adding modified nano white carbon black, an organic phosphate flame retardant, a phosphorus-nitrogen flame retardant powder mixture and a smoke suppressor, and continuously circulating for 1 hour; homogenizing, degassing, and transferring into a finished product tank.
Example 3
The embodiment provides an environment-friendly flame-retardant water-blocking paste, which comprises the following components in the formula table 3:
TABLE 3 Table 3
Component \ Content of
Modified sodium bentonite 3.6
Modified silica gel 4
Trimellitic acid ester 32
Pentaerythritol esters 22.4
Hydrogenated styrene-isoprene copolymer 10
Propylene carbonate 1.2
Modified nano white carbon black 2.5
2, 6-Di-tert-butyl-p-cresol 0.8
Neutral barium dinonyl naphthalene sulfonate 0.7
Ethylene oxide/propylene oxide block copolyethers 0.3
Organic phosphate flame retardant 17
Phosphorus-nitrogen flame retardant powder mixture 3.5
Smoke eliminator 2
Wherein, the modified sodium bentonite adopts Zhejiang Hongyu new material Co., ltd, and the product with the code HY 738; the modified silica gel adopts Shenzhen Jin Wang Keji Co., ltd, code JW-E600 product; pentaerythritol ester is a POE320 product of Yingkou star fire chemical industry Co., ltd; the hydrogenated styrene-isoprene copolymer adopts the product with the code SEP YH-4010 of the petrochemical company, basil, china petrochemical Co., ltd; modified nano white carbon black adopts a product of Weifang constant scintillation nano material limited company, code HS-9280; the ethylene oxide/propylene oxide block copolyether adopts a product with the code DL-32 of Qingdao Sofu wetting chemical engineering Co., ltd; the organic phosphate flame retardant adopts Nanjing Sier chemical production, and the product is named HR-105; the phosphorus-nitrogen flame retardant powder mixture is produced by Nanjing Sier chemical industry, and the product is named HR-202; the smoke suppressor is ferrocene: zinc molybdate: melamine hydroxystannate and zinc hydroxystannate in the mass ratio of 1:2:1:1.
The preparation method of the environment-friendly flame-retardant water-blocking paste comprises the following steps:
(1) Mixing base oil of trimellitate and pentaerythritol ester according to a proportion, and pumping the base oil into a fat manufacturing kettle; heating to 60 ℃, adding the hydrogenated styrene-isoprene copolymer, continuously stirring and heating to 170 ℃, and transferring into a blending kettle.
(2) Adding modified silica gel into the blending kettle, and stirring for 30 minutes; and (3) opening water cooling, cooling to 135 ℃, closing the water cooling, adding the modified sodium bentonite and the propylene carbonate, opening a circulating shearing machine, adjusting the shearing pressure to 1.1MPa, and shearing for 3 hours after the modified sodium bentonite and the propylene carbonate are completely dispersed.
(3) And (3) opening a water-cooling device, cooling to 75 ℃, sequentially adding an antioxidant, an antirust agent and a demulsifier, continuously circularly shearing for 1 hour, and then reducing the shearing pressure to zero.
(4) Sequentially adding modified nano white carbon black, an organic phosphate flame retardant, a phosphorus-nitrogen flame retardant powder mixture and a smoke suppressor, and continuously circulating for 1 hour; homogenizing, degassing, and transferring into a finished product tank.
Example 4
The embodiment provides an environment-friendly flame-retardant water-blocking paste, which comprises the following components in the formula table 4:
TABLE 4 Table 4
Component \ Content of
Modified sodium bentonite 3.7
Modified silica gel 3.5
Trimellitic acid ester 31
Pentaerythritol esters 23.9
Hydrogenated styrene-isoprene copolymer 9
Propylene carbonate 1
Modified nano white carbon black 2.5
2, 6-Di-tert-butyl-p-cresol 0.8
Neutral barium dinonyl naphthalene sulfonate 0.8
Ethylene oxide/propylene oxide block copolyethers 0.3
Organic phosphate flame retardant 17.5
Phosphorus-nitrogen flame retardant powder mixture 3.5
Smoke eliminator 2.5
Wherein, the modified sodium bentonite adopts Zhejiang Hongyu new material Co., ltd, and the product with the code HY 738; the modified silica gel adopts Shenzhen Jin Wang Keji Co., ltd, code JW-E600 product; pentaerythritol ester is a POE320 product of Yingkou star fire chemical industry Co., ltd; the hydrogenated styrene-isoprene copolymer adopts the product with the code SEP YH-4010 of the petrochemical company, basil, china petrochemical Co., ltd; modified nano white carbon black adopts a product of Weifang constant scintillation nano material limited company, code HS-9280; the ethylene oxide/propylene oxide block copolyether adopts a product with the code DL-32 of Qingdao Sofu wetting chemical engineering Co., ltd; the organic phosphate flame retardant adopts Nanjing Sier chemical production, and the product is named HR-105; the phosphorus-nitrogen flame retardant powder mixture is produced by Nanjing Sier chemical industry, and the product is named HR-202; the smoke suppressor is ferrocene: zinc molybdate: melamine hydroxystannate and zinc hydroxystannate in the mass ratio of 1:2:1:1.
The preparation method of the environment-friendly flame-retardant water-blocking paste comprises the following steps:
(1) Mixing base oil of trimellitate and pentaerythritol ester according to a proportion, and pumping the base oil into a fat manufacturing kettle; heating to 60 ℃, adding the hydrogenated styrene-isoprene copolymer, continuously stirring and heating to 170 ℃, and transferring into a blending kettle.
(2) Adding modified silica gel into the blending kettle, and stirring for 30 minutes; and (3) opening water cooling, cooling to 135 ℃, closing the water cooling, adding the modified sodium bentonite and the propylene carbonate, opening a circulating shearing machine, adjusting the shearing pressure to 1.1MPa, and shearing for 3 hours after the modified sodium bentonite and the propylene carbonate are completely dispersed.
(3) And (3) opening a water-cooling device, cooling to 75 ℃, sequentially adding an antioxidant, an antirust agent and a demulsifier, continuously circularly shearing for 1 hour, and then reducing the shearing pressure to zero.
(4) Sequentially adding modified nano white carbon black, an organic phosphate flame retardant, a phosphorus-nitrogen flame retardant powder mixture and a smoke suppressor, and continuously circulating for 1 hour; homogenizing, degassing, and transferring into a finished product tank.
Comparative example 1
The comparative example provides an environment-friendly flame-retardant water-blocking paste, which comprises the following components in the formula table 5:
TABLE 5
Figure BDA0003105678830000131
Figure BDA0003105678830000141
Wherein, the modified silica gel adopts Shenzhen gold Wang Keji Co., ltd, code JW-E600 product; pentaerythritol ester is a POE320 product of Yingkou star fire chemical industry Co., ltd; the hydrogenated styrene-isoprene copolymer adopts the product with the code SEP YH-4010 of the petrochemical company, basil, china petrochemical Co., ltd; modified nano white carbon black adopts a product of Weifang constant scintillation nano material limited company, code HS-9280; the ethylene oxide/propylene oxide block copolyether adopts a product with the code DL-32 of Qingdao Sofu wetting chemical engineering Co., ltd; the organic phosphate flame retardant adopts Nanjing Sier chemical production, and the product is named HR-105; the phosphorus-nitrogen flame retardant powder mixture is produced by Nanjing Sier chemical industry, and the product is named HR-202; the smoke suppressor is ferrocene: zinc molybdate: melamine hydroxystannate and zinc hydroxystannate in the mass ratio of 1:2:1:1.
The preparation method of the environment-friendly flame-retardant water-blocking paste comprises the following steps:
(1) Mixing base oil of trimellitate and pentaerythritol ester according to a proportion, and pumping the base oil into a fat manufacturing kettle; heating to 60 ℃, adding the hydrogenated styrene-isoprene copolymer, continuously stirring and heating to 170 ℃, and transferring into a blending kettle.
(2) Adding modified silica gel into the blending kettle, and stirring for 30 minutes; and (3) opening water cooling, cooling to 135 ℃, closing the water cooling, adding propylene carbonate, opening a circulating shearing machine after the propylene carbonate is completely dispersed, adjusting the shearing pressure to 1.1MPa, and shearing for 3 hours.
(3) And (3) opening a water-cooling device, cooling to 75 ℃, sequentially adding an antioxidant, an antirust agent and a demulsifier, continuously circularly shearing for 1 hour, and then reducing the shearing pressure to zero.
(4) Sequentially adding modified nano white carbon black, an organic phosphate flame retardant, a phosphorus-nitrogen flame retardant powder mixture and a smoke suppressor, and continuously circulating for 1 hour; homogenizing, degassing, and transferring into a finished product tank.
Comparative example 2
The comparative example provides an environment-friendly flame-retardant water-blocking paste, which comprises the following components in the formula table 6:
TABLE 6
Figure BDA0003105678830000142
Figure BDA0003105678830000151
Wherein, the modified sodium bentonite adopts Zhejiang Hongyu new material Co., ltd, and the product with the code HY 738; the modified silica gel adopts Shenzhen Jin Wang Keji Co., ltd, code JW-E600 product; the metallocene polydiene copolymer is a product with the code Daelimsynol 40 of Shanghai's Ind chemical industry Co-Ltd; the hydrogenated styrene-isoprene copolymer adopts the product with the code SEP YH-4010 of the petrochemical company, basil, china petrochemical Co., ltd; modified nano white carbon black adopts a product of Weifang constant scintillation nano material limited company, code HS-9280; the ethylene oxide/propylene oxide block copolyether adopts a product with the code DL-32 of Qingdao Sofu wetting chemical engineering Co., ltd; the organic phosphate flame retardant adopts Nanjing Sier chemical production, and the product is named HR-105; the phosphorus-nitrogen flame retardant powder mixture is produced by Nanjing Sier chemical industry, and the product is named HR-202; the smoke suppressor is ferrocene: zinc molybdate: melamine hydroxystannate and zinc hydroxystannate in the mass ratio of 1:2:1:1.
The preparation method of the environment-friendly flame-retardant water-blocking paste comprises the following steps:
(1) According to the proportion, the metallocene polydiene copolymer is pumped into a fat-making kettle; heating to 60 ℃, adding the hydrogenated styrene-isoprene copolymer, continuously stirring and heating to 170 ℃, and transferring into a blending kettle.
(2) Adding modified silica gel into the blending kettle, and stirring for 30 minutes; and (3) opening water cooling, cooling to 1305 ℃, closing the water cooling, adding the modified sodium bentonite and the propylene carbonate, opening a circulating shearing machine, adjusting the shearing pressure to 1.1MPa, and shearing for 3 hours after the modified sodium bentonite and the propylene carbonate are completely dispersed.
(3) And (3) opening a water-cooling device, cooling to 75 ℃, sequentially adding an antioxidant, an antirust agent and a demulsifier, continuously circularly shearing for 1 hour, and then reducing the shearing pressure to zero.
(4) Sequentially adding modified nano white carbon black, an organic phosphate flame retardant, a phosphorus-nitrogen flame retardant powder mixture and a smoke suppressor, and continuously circulating for 1 hour; homogenizing, degassing, and transferring into a finished product tank.
Comparative example 3
The comparative example provides an environment-friendly flame-retardant water-blocking paste, which comprises the following components in the formula table 7:
TABLE 4 Table 4
Component \ Content of
Modified sodium bentonite 3.7
Modified silica gel 3.5
Trimellitic acid ester 31
Pentaerythritol esters 23.9
Hydrogenated styrene-isoprene copolymer 9
Propylene carbonate 1
Modified nano white carbon black 2.5
2, 6-Di-tert-butyl-p-cresol 0.8
Neutral barium dinonyl naphthalene sulfonate 0.8
Organic phosphate flame retardant 17.5
Phosphorus-nitrogen flame retardant powder mixture 3.5
Smoke eliminator 2.5
Wherein, the modified sodium bentonite adopts Zhejiang Hongyu new material Co., ltd, and the product with the code HY 738; the modified silica gel adopts Shenzhen Jin Wang Keji Co., ltd, code JW-E600 product; pentaerythritol ester is a POE320 product of Yingkou star fire chemical industry Co., ltd; the hydrogenated styrene-isoprene copolymer adopts the product with the code SEP YH-4010 of the petrochemical company, basil, china petrochemical Co., ltd; modified nano white carbon black adopts a product of Weifang constant scintillation nano material limited company, code HS-9280; the organic phosphate flame retardant adopts Nanjing Sier chemical production, and the product is named HR-105; the phosphorus-nitrogen flame retardant powder mixture is produced by Nanjing Sier chemical industry, and the product is named HR-202; the smoke suppressor is ferrocene: zinc molybdate: melamine hydroxystannate and zinc hydroxystannate in the mass ratio of 1:2:1:1.
The preparation method of the environment-friendly flame-retardant water-blocking paste comprises the following steps:
(1) Mixing base oil of trimellitate and pentaerythritol ester according to a proportion, and pumping the base oil into a fat manufacturing kettle; heating to 60 ℃, adding the hydrogenated styrene-isoprene copolymer, continuously stirring and heating to 170 ℃, and transferring into a blending kettle.
(2) Adding modified silica gel into the blending kettle, and stirring for 30 minutes; and (3) opening water cooling, cooling to 135 ℃, closing the water cooling, adding the modified sodium bentonite and the propylene carbonate, opening a circulating shearing machine, adjusting the shearing pressure to 1.1MPa, and shearing for 3 hours after the modified sodium bentonite and the propylene carbonate are completely dispersed.
(3) And (3) opening a water-cooling device, cooling to 75 ℃, sequentially adding an antioxidant and an antirust agent, continuously circularly shearing for 1 hour, and then reducing the shearing pressure to zero.
(4) Sequentially adding modified nano white carbon black, an organic phosphate flame retardant, a phosphorus-nitrogen flame retardant powder mixture and a smoke suppressor, and continuously circulating for 1 hour; homogenizing, degassing, and transferring into a finished product tank.
Comparative example 4
The comparative example provides an environment-friendly flame-retardant water-blocking paste, which comprises the following components in the formula table 8:
TABLE 8
Component \ Content of
Modified sodium bentonite 3.7
Modified silica gel 12.5
Trimellitic acid ester 31
Pentaerythritol esters 23.9
Propylene carbonate 1
Modified nano white carbon black 2.5
2, 6-Di-tert-butyl-p-cresol 0.8
Neutral barium dinonyl naphthalene sulfonate 0.8
Ethylene oxide/propylene oxide block copolyethers 0.3
Organic phosphate flame retardant 17.5
Phosphorus-nitrogen flame retardant powder mixture 3.5
Smoke eliminator 2.5
Wherein, the modified sodium bentonite adopts Zhejiang Hongyu new material Co., ltd, and the product with the code HY 738; the modified silica gel adopts Shenzhen Jin Wang Keji Co., ltd, code JW-E600 product; pentaerythritol ester is a POE320 product of Yingkou star fire chemical industry Co., ltd; modified nano white carbon black adopts a product of Weifang constant scintillation nano material limited company, code HS-9280; the ethylene oxide/propylene oxide block copolyether adopts a product with the code DL-32 of Qingdao Sofu wetting chemical engineering Co., ltd; the organic phosphate flame retardant adopts Nanjing Sier chemical production, and the product is named HR-105; the phosphorus-nitrogen flame retardant powder mixture is produced by Nanjing Sier chemical industry, and the product is named HR-202; the smoke suppressor is ferrocene: zinc molybdate: melamine hydroxystannate and zinc hydroxystannate in the mass ratio of 1:2:1:1.
The preparation method of the environment-friendly flame-retardant water-blocking paste comprises the following steps:
(1) Mixing base oil of trimellitate and pentaerythritol ester according to a proportion, and pumping the base oil into a fat manufacturing kettle; heating to 60 ℃ and stirring, continuously stirring and heating to 170 ℃, and transferring into a blending kettle.
(2) Adding modified silica gel into the blending kettle, and stirring for 30 minutes; and (3) opening water cooling, cooling to 135 ℃, closing the water cooling, adding the modified sodium bentonite and the propylene carbonate, opening a circulating shearing machine, adjusting the shearing pressure to 1.1MPa, and shearing for 3 hours after the modified sodium bentonite and the propylene carbonate are completely dispersed.
(3) And (3) opening a water-cooling device, cooling to 75 ℃, sequentially adding an antioxidant, an antirust agent and a demulsifier, continuously circularly shearing for 1 hour, and then reducing the shearing pressure to zero.
(4) Sequentially adding modified nano white carbon black, an organic phosphate flame retardant, a phosphorus-nitrogen flame retardant powder mixture and a smoke suppressor, and continuously circulating for 1 hour; homogenizing, degassing, and transferring into a finished product tank.
Comparative example 5
The comparative example provides an environment-friendly flame-retardant water-blocking paste, which comprises the following components in the formula table 9:
TABLE 9
Component \ Content of
Modified sodium bentonite 3.7
Modified silica gel 3.5
Trimellitic acid ester 31
Pentaerythritol esters 23.9
Hydrogenated styrene-isoprene copolymer 9
Propylene carbonate 1
Modified nano white carbon black 2.5
2, 6-Di-tert-butyl-p-cresol 0.8
Neutral barium dinonyl naphthalene sulfonate 0.8
Ethylene oxide/propylene oxide block copolyethers 0.3
Organic phosphate flame retardant 17.5
Phosphorus-nitrogen flame retardant powder mixture 3.5
Wherein, the modified sodium bentonite adopts Zhejiang Hongyu new material Co., ltd, and the product with the code HY 738; the modified silica gel adopts Shenzhen Jin Wang Keji Co., ltd, code JW-E600 product; pentaerythritol ester is a POE320 product of Yingkou star fire chemical industry Co., ltd; the hydrogenated styrene-isoprene copolymer adopts the product with the code SEP YH-4010 of the petrochemical company, basil, china petrochemical Co., ltd; modified nano white carbon black adopts a product of Weifang constant scintillation nano material limited company, code HS-9280; the ethylene oxide/propylene oxide block copolyether adopts a product with the code DL-32 of Qingdao Sofu wetting chemical engineering Co., ltd; the organic phosphate flame retardant adopts Nanjing Sier chemical production, and the product is named HR-105; the phosphorus-nitrogen flame retardant powder mixture is produced by Nanjing Sier chemical industry, and the code is HR-202.
The preparation method of the environment-friendly flame-retardant water-blocking paste comprises the following steps:
(1) Mixing base oil of trimellitate and pentaerythritol ester according to a proportion, and pumping the base oil into a fat manufacturing kettle; heating to 60 ℃, adding the hydrogenated styrene-isoprene copolymer, continuously stirring and heating to 170 ℃, and transferring into a blending kettle.
(2) Adding modified silica gel into the blending kettle, and stirring for 30 minutes; and (3) opening water cooling, cooling to 135 ℃, closing the water cooling, adding the modified sodium bentonite and the propylene carbonate, opening a circulating shearing machine, adjusting the shearing pressure to 1.1MPa, and shearing for 3 hours after the modified sodium bentonite and the propylene carbonate are completely dispersed.
(3) And (3) opening a water-cooling device, cooling to 75 ℃, sequentially adding an antioxidant, an antirust agent and a demulsifier, continuously circularly shearing for 1 hour, and then reducing the shearing pressure to zero.
(4) Sequentially adding the modified nano white carbon black, the organic phosphate flame retardant and the phosphorus-nitrogen flame retardant powder mixture, and continuously circulating for 1 hour; homogenizing, degassing, and transferring into a finished product tank.
Comparative example 6
The comparative example provides an environment-friendly flame-retardant water-blocking paste, which comprises the following components in the formula table 10:
table 10
Figure BDA0003105678830000191
Figure BDA0003105678830000201
Wherein, the modified sodium bentonite adopts Zhejiang Hongyu new material Co., ltd, and the product with the code HY 738; the modified silica gel adopts Shenzhen Jin Wang Keji Co., ltd, code JW-E600 product; pentaerythritol ester is a POE320 product of Yingkou star fire chemical industry Co., ltd; the hydrogenated styrene-isoprene copolymer adopts the product with the code SEP YH-4010 of the petrochemical company, basil, china petrochemical Co., ltd; the ethylene oxide/propylene oxide block copolyether adopts a product with the code DL-32 of Qingdao Sofu wetting chemical engineering Co., ltd; the organic phosphate flame retardant adopts Nanjing Sier chemical production, and the product is named HR-105; the phosphorus-nitrogen flame retardant powder mixture is produced by Nanjing Sier chemical industry, and the product is named HR-202; the smoke suppressor is ferrocene: zinc molybdate: melamine hydroxystannate and zinc hydroxystannate in the mass ratio of 1:2:1:1.
The preparation method of the environment-friendly flame-retardant water-blocking paste comprises the following steps:
(1) Mixing base oil of trimellitate and pentaerythritol ester according to a proportion, and pumping the base oil into a fat manufacturing kettle; heating to 60 ℃, adding the hydrogenated styrene-isoprene copolymer, continuously stirring and heating to 170 ℃, and transferring into a blending kettle.
(2) Adding modified silica gel into the blending kettle, and stirring for 30 minutes; and (3) opening water cooling, cooling to 135 ℃, closing the water cooling, adding the modified sodium bentonite and the propylene carbonate, opening a circulating shearing machine, adjusting the shearing pressure to 1.1MPa, and shearing for 3 hours after the modified sodium bentonite and the propylene carbonate are completely dispersed.
(3) And (3) opening a water-cooling device, cooling to 75 ℃, sequentially adding an antioxidant, an antirust agent and a demulsifier, continuously circularly shearing for 1 hour, and then reducing the shearing pressure to zero.
(4) Sequentially adding an organic phosphate flame retardant, a phosphorus-nitrogen flame retardant powder mixture and a smoke suppressor, and continuously circulating for 1 hour; homogenizing, degassing, and transferring into a finished product tank.
Performance testing
The applicant has carried out the following performance tests on the preservative grease samples in the above examples and comparative examples, see table 11 below for specific experimental items and test criteria:
table 11 test items and test criteria
Figure BDA0003105678830000202
Figure BDA0003105678830000211
Wherein:
and (b) the following steps: DC1000V, stylus contacts were inserted into the sample at intervals of 10mm,60s, insulation 500MΩ.
And b: AC2500, stylus contacts were inserted into the sample at intervals of 10mm,60s, leakage current 1mA.
And c: placing 10g of a sample under the flame for 10s, removing the flame, extinguishing for 10s, placing the sample under the flame for 10s, removing the flame, and extinguishing for 10 s; while less smoke is visually observed.
Table 12 results of performance tests
Test item Example 1 Example 2 Example 3 Example 4 Comparative example 1
The penetration (25 ℃,150 g) of the non-working cone is 1/10mm 323 328 331 319 329
The penetration of the working cone (-40 ℃,150 g) is 1/10mm 128 132 135 130 143
Drop point (DEG C) 254 258 248 256 245
Flash point (DEG C) 292 294 292 296 292
Steel mesh oil separation (80 ℃,24 h)/wt% 0 0 0 0 0.4
Evaporation capacity (80 ℃,24 h)/wt% 0 0 0 0 0.1
Water resistance (23 ℃,7 x 24 h) Not disintegrate Not disintegrate Not disintegrate Not disintegrate Not disintegrate
Insulation test (attached a) By passing through By passing through By passing through By passing through By passing through
Withstand voltage test (with b) By passing through By passing through By passing through By passing through By passing through
Flame retardant smoke abatement test (with c) By passing through By passing through By passing through By passing through By passing through
Test item Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5 Comparative example 6
The penetration (25 ℃,150 g) of the non-working cone is 1/10mm 320 319 341 320 338
The penetration of the working cone (-40 ℃,150 g) is 1/10mm 148 138 147 130 146
Drop point (DEG C) 254 251 242 257 246
Flash point (DEG C) 296 291 290 295 290
Steel mesh oil separation (80 ℃,24 h)/wt% 0 0.5 1.4 0 1.1
Evaporation capacity (80 ℃,24 h)/wt% 0 0.3 0.8 0 0.6
Water resistance (23 ℃,7 x 24 h) Not disintegrate Disintegration of Disintegration of Not disintegrate Disintegration of
Insulation test (attached a) By passing through By passing through Not pass through By passing through Not pass through
Withstand voltage test (with b) By passing through By passing through Not pass through Not pass through Not pass through
Flame retardant smoke abatement test (with c) By passing through By passing through By passing through Not pass through By passing through
From the experimental results, the environment-friendly flame-retardant water-blocking paste has excellent wide-temperature applicability; as can be seen from the water resistance test data in the table, the filling paste provided by the invention is not disintegrated after 7 days of test, which proves that the filling paste provided by the invention has good water resistance. As can be seen from the insulation voltage test data in the table, the filling paste provided by the invention has good electrical property; as can be seen from the flame-retardant test in the table, the filling paste does not have excessive black smoke after flame burning, which proves that the filling paste provided by the invention has excellent flame-retardant smoke-eliminating property.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention in any way; those skilled in the art will readily appreciate that the present invention is well adapted to carry out the ends of the same out as described herein; however, those skilled in the art will appreciate that many modifications, adaptations, and variations of the present invention are possible in light of the above teachings without departing from the scope of the invention; meanwhile, any equivalent changes, modifications and evolution of the above embodiments according to the essential technology of the present invention still fall within the scope of the present invention.

Claims (3)

1. The environment-friendly flame-retardant water-blocking paste is characterized by comprising the following raw materials in parts by weight:
1 to 6 portions of inorganic thickening agent
Gelling agent 8-20
Base oil 30-70
12 to 30 portions of flame retardant
3-12 of other auxiliary agents;
the inorganic thickening agent is quaternary ammonium salt modified sodium bentonite, and accounts for 3-4wt% of the total amount of the preparation raw materials of the environment-friendly flame-retardant water-blocking paste;
the gellant comprises a hydrogenated styrene-isoprene copolymer; the content of the hydrogenated styrene-isoprene copolymer accounts for 6-12 wt% of the total amount of the raw materials for preparing the environment-friendly flame-retardant water-blocking paste;
the gelling agent further comprises a modified silica gel;
the base oil comprises trimellitate and pentaerythritol ester, wherein the mass ratio of the trimellitate to the pentaerythritol ester is (25-35): (15-24), the kinematic viscosity of the pentaerythritol ester at 100 ℃ is 27-30 mm 2 /s；
The flame retardant is a mixture of organic phosphate liquid flame retardant and phosphorus-nitrogen flame retardant powder flame retardant;
the other auxiliary agents comprise propylene carbonate and modified nano white carbon black, and the total addition amount of the propylene carbonate and the modified nano white carbon black is any one of 3 parts, 3.1 parts, 3.5 parts and 3.7 parts;
the other auxiliary agent comprises demulsifier ethylene oxide/propylene oxide block copolyether;
The other auxiliary agent comprises a smoke suppressor; the smoke suppressor consists of ferrocene, zinc molybdate, melamine hydroxy stannate and zinc hydroxystannate, and the weight ratio is 1:2:1:1;
the other auxiliary agents also comprise an antioxidant 2, 6-di-tert-butyl-p-cresol;
the other auxiliary agents also comprise rust inhibitor neutral barium dinonyl naphthalene sulfonate.
2. The method for preparing the environment-friendly flame-retardant water-blocking paste according to claim 1, which is characterized by comprising the following steps:
(1) According to the proportion, the base oil is pumped into a fat making kettle, the temperature is raised to 50-70 ℃, the gelatinizing agent is added, the stirring and the temperature are continuously raised to 160-180 ℃, and the base oil is transferred into a blending kettle;
(2) Cooling the raw materials of the blending kettle to 130-140 ℃, adding an inorganic thickening agent, and circulating a shearing machine for 2-4 hours, wherein the shearing pressure is regulated to 1.0-1.2 MPa;
(3) Then cooling to 70-80 ℃, adding other auxiliary agents, continuously circularly shearing for 0.5-2 hours, reducing the shearing pressure to zero, adding the rest raw materials, continuously stirring and circularly recycling for 1 hour, and finally obtaining the finished product.
3. The application of the environment-friendly flame-retardant water-blocking paste according to claim 1, which is applied to the technical field of communication optical cables.
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