High boiling point treatment method

Abstract

The present invention provides a method for treating high-boiling substances, including those discharged from a silicate production process. The method comprises: subjecting the high-boiling substances to a hydrolysis reaction under the action of a catalyst, followed by a first solid-liquid separation to obtain a first solid-phase product and a first filtrate, respectively; wherein the catalyst comprises an acid; adjusting the pH of the first filtrate to 6-10, sequentially performing a crystallization process and a second solid-liquid separation to obtain a second solid-phase product and a second filtrate, respectively; distilling the second filtrate to obtain an organic phase and an aqueous phase, respectively; and returning the aqueous phase to participate in the hydrolysis reaction. The present invention can efficiently recycle high-boiling substances discharged from the silicate production process and has the advantages of a simple treatment process, low energy consumption, and avoidance of secondary pollution.

Description

Technical Field

[0001] The invention relates to the recycling of emissions from a silicate production process, and in particular to a high-boiling-point treatment method. Background Art

[0002] During the synthesis of silicates, high-boiling substances are discharged. These high-boiling substances mainly include unreacted raw materials such as organic alcohols, as well as by-products such as polysilicates and other high-molecular organic substances produced due to side reactions. The efficient recovery and utilization of high-boiling substances is of great significance for improving the raw material utilization rate and reducing costs in the silicate production process.

[0003] At present, there are two main methods for treating high-boiling substances: (1) separating the high-boiling substances into components, specifically strictly separating the components by distillation. This process usually requires a high-temperature heat source to vaporize the high-boiling substances and then condense and separate them. The process is complicated, energy-intensive, and has high processing costs, which is not conducive to practical application; (2) incinerating the high-boiling substances. However, this consumes a lot of fuel, increases carbon emissions, causes secondary pollution, increases environmental pressure, and is not conducive to practical application.

[0004] Therefore, developing a new high-boiling-point treatment process, especially suitable for efficiently recovering high-boiling-point discharges from silicate production processes, and simplifying the treatment process, reducing energy consumption, and avoiding secondary pollution, is still a technical problem faced by those skilled in the art. Summary of the Invention

[0005] The present invention provides a high-boiling-point substance treatment method, which can efficiently recycle high-boiling-point substances discharged from a silicate production process, and has the advantages of simple treatment process, low energy consumption, and avoidance of secondary pollution.

[0006] The present invention provides a method for treating high-boiling substances, wherein the high-boiling substances include high-boiling substances discharged from a silicate production process. The method comprises: subjecting the high-boiling substances to a hydrolysis reaction under the action of a catalyst, and then subjecting the high-boiling substances to a first solid-liquid separation to obtain a first solid-phase product and a first filtrate, respectively; wherein the catalyst comprises an acid; adjusting the pH of the first filtrate to 6-10, and sequentially performing a crystallization treatment and a second solid-liquid separation to obtain a second solid-phase product and a second filtrate, respectively; distilling the second filtrate to obtain an organic phase and an aqueous phase, respectively; and returning at least a portion of the aqueous phase to participate in the hydrolysis reaction.

[0007] According to one embodiment of the present invention, the high boiling substances include polysilicate and organic alcohol.

[0008] According to one embodiment of the present invention, the acid comprises an inorganic acid.

[0009] According to one embodiment of the present invention, the inorganic acid includes hydrochloric acid and / or sulfuric acid.

[0010] According to one embodiment of the present invention, the hydrolysis reaction time is 30 minutes to 120 minutes; and / or, during the hydrolysis reaction, a first agitator is used for stirring, and the first agitator includes a paddle agitator and / or an anchor agitator.

[0011] According to one embodiment of the present invention, the first solid-liquid separation is performed by filtration with a filtration accuracy of 100 nm to 600 nm to obtain the first solid phase product and the first filtrate; and / or the first solid phase product includes silicon dioxide.

[0012] According to one embodiment of the present invention, alkali is added to the first filtrate to adjust the pH of the first filtrate to 6-10, and the alkali includes potassium hydroxide and / or sodium hydroxide.

[0013] According to one embodiment of the present invention, the crystallization treatment is performed at a temperature of 5°C to 40°C.

[0014] According to one embodiment of the present invention, during the crystallization treatment, a second agitator is used for stirring, and the second agitator includes a paddle agitator and / or an anchor agitator. The stirring time is 30 minutes to 60 minutes.

[0015] According to one embodiment of the present invention, the organic phase includes organic alcohol; and / or the mass percentage of water in the organic phase is 0.01% to 0.1%.

[0016] In the present invention, high-boiling substances are hydrolyzed under the action of acid, and the subsequent first solid-liquid separation, adjustment of the pH of the first filtrate to 6-8, crystallization treatment, second solid-liquid separation, distillation of the second filtrate, and return of the aqueous phase to participate in the hydrolysis reaction are combined to achieve the recovery and utilization of high-boiling substances. Moreover, the treatment process does not require strict separation of the components in the high-boiling substances and does not require combustion of the high-boiling substances. The process is simple and energy consumption is low. At the same time, no wastewater or hazardous solid waste is generated during the treatment process, which is safer and more environmentally friendly, reduces environmental pressure, and is of great significance for practical industrial applications. Therefore, the present application can efficiently recycle high-boiling substances discharged from the silicate production process, and the organic phase produced by distillation can be used as a raw material for silicate production, thereby improving the utilization rate of raw materials in the silicate production process. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 Schematic diagram of the structure of a high boiling point processing device according to an embodiment of the present invention.

[0018] Explanation of the reference numerals: 1: hydrolysis reactor; 10: first cavity; 11: first shell; 101: first stirring part; 102: first stirring rod; 103: first motor; 2: first filter; 3: crystallizer; 30: second cavity; 31: second shell; 301: second stirring part; 302: second stirring rod; 303: second motor; 4: cooling system; 40: third cavity; 41: side wall; 42: bottom wall; 5: second filter; 6: distillation tower; 601: condenser; 602: reboiler; a: high boiling point; b: water; c: catalyst; d: hydrolysis mixture; e: first solid phase product; f: first filtrate; g: pH regulator; h: crystallization mixture; i: second solid phase product; j: second filtrate; k: organic phase; n: aqueous phase. DETAILED DESCRIPTION

[0019] In order to enable those skilled in the art to better understand the scheme of the present invention, the present invention is further described in detail below. The specific embodiments listed below are only for describing the principles and features of the present invention. The examples are only used to explain the present invention and are not intended to limit the scope of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts are within the scope of protection of the present invention.

[0020] In the description of the present invention, unless otherwise clearly specified and limited, the terms "set", "connect", and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection, an electrical connection, or a communication connection (network connection); it can be a direct connection, an indirect connection through an intermediate medium, or the two elements can be internally connected. For ordinary technicians in this field, the specific meanings of the above-mentioned terms in the present invention can be understood according to the specific circumstances. In addition, terms such as "first" and "second" are only used for descriptive purposes, such as distinguishing between components to more clearly illustrate / explain the technical solution, and cannot be understood as indicating or implying the number of the indicated technical features or the order of substantial significance.

[0021] The embodiment of the present invention provides a method for treating high boiling points, such as Figure 1 As shown, the high-boiling substance a includes high-boiling substances discharged from a silicate production process, and a method for treating the high-boiling substance a includes: subjecting the high-boiling substance a to a hydrolysis reaction under the action of a catalyst c, followed by a first solid-liquid separation to obtain a first solid-phase product e and a first filtrate f, respectively; wherein the catalyst c includes an acid; adjusting the pH of the first filtrate f to 6-10, sequentially performing a crystallization treatment and a second solid-liquid separation to obtain a second solid-phase product i and a second filtrate j, respectively; distilling the second filtrate j to obtain an organic phase k and an aqueous phase n, respectively; and returning at least a portion of the aqueous phase n to participate in the hydrolysis reaction.

[0022] The high boiling substances a are high boiling substances discharged from the silicate production process, and the high boiling substances a may specifically include high molecular organic substances such as organic alcohols and polysilicates.

[0023] In the above treatment process, an acid is used as a catalyst c to catalyze the hydrolysis of the high-boiling substance a. The acid used may specifically include an inorganic acid, and in particular may include hydrochloric acid and / or sulfuric acid.

[0024] Specifically, the hydrolysis reaction is carried out in the presence of water. During specific implementation, the hydrolysis reaction can be carried out in a mixed system containing a high boiling point substance a, a catalyst c, and water b. For example, the high boiling point substance a, the catalyst c, and the water b can be mixed to form the mixed system for carrying out the hydrolysis reaction; alternatively, the high boiling point substance a and an aqueous solution of the catalyst c (or a liquid catalyst, such as an acid aqueous solution) can be mixed to form the mixed system for carrying out the hydrolysis reaction, that is, the high boiling point substance a can be added to an aqueous solution of the catalyst c to carry out the hydrolysis reaction; alternatively, the high boiling point substance a, an aqueous solution of the catalyst c, and the water b can be mixed to form the mixed system for carrying out the hydrolysis reaction.

[0025] The acid aqueous solution includes, for example, dilute hydrochloric acid and / or dilute sulfuric acid. For example, the high boiling point a can be added to dilute hydrochloric acid, dilute sulfuric acid, or a mixture of dilute hydrochloric acid and dilute sulfuric acid to carry out a hydrolysis reaction.

[0026] In addition, if Figure 1 As shown, the above-mentioned hydrolysis reaction can be carried out under stirring, that is, during the above-mentioned hydrolysis reaction, the first agitator can be used to stir the above-mentioned mixed system. The first agitator can specifically include a paddle agitator and / or an anchor agitator, and a paddle agitator is usually preferred. In this way, the high boiling point a is fully contacted with the catalyst c, so that the high boiling point a is completely hydrolyzed.

[0027] When implementing it specifically, Figure 1 As shown, the hydrolysis reaction can be carried out in a conventional device in the art such as a hydrolysis reactor (or hydrolysis kettle) 1. The high boiling point a is transported to the hydrolysis kettle, the stirrer is turned on for stirring, and then the required materials such as the catalyst c and water b are added thereto in sequence. The stirring is then maintained for 30 to 120 minutes (i.e., the hydrolysis reaction time) to complete the hydrolysis reaction.

[0028] Specifically, the hydrolysis reaction time can be 30 to 120 minutes (min), for example, 30 minutes, 40 minutes, 50 minutes, 60 minutes, 70 minutes, 80 minutes, 90 minutes, 100 minutes, 110 minutes, 120 minutes or a range consisting of any two thereof.

[0029] The high-boiling product a is hydrolyzed by the hydrolysis reaction, and then separated by a first solid-liquid separation to produce a first solid phase product e and a first filtrate f. The first solid phase product e is typically silicon dioxide, a harmless solid product that can be used as an industrial raw material.

[0030] Specifically, the first solid-liquid separation can be carried out by filtration, that is, the system after the hydrolysis reaction is filtered to obtain a first solid phase product e and a first filtrate f, respectively, wherein the filtration accuracy can be 100nm to 600nm, for example, 100nm, 150nm, 200nm, 250nm, 300nm, 350nm, 400nm, 450nm, 500nm, 550nm, 600nm or a range consisting of any two of them.

[0031] In a specific implementation, the system after the hydrolysis reaction (hydrolysis mixture d) can be filtered (i.e., the first solid-liquid separation) using the first filter 2, that is, the system after the hydrolysis reaction enters the first filter 2 for filtration to obtain a first solid phase product e and a first filtrate f, respectively. In the embodiment of the present invention, conventional filters in the art can be used as the first filter 2, and there is no particular limitation on this.

[0032] Among them, the filtration accuracy refers to the pore size of the filter element (filter mesh) of the filter, which is also the size of the maximum particles allowed to pass through the filter element when the system to be filtered passes through the filter element. That is, the filtration accuracy as mentioned above can be 100nm~600nm, which means that the mixture d after hydrolysis is filtered through the filter element in the first filter 2 (i.e., the first solid-liquid separation), and the size of the maximum solid particles (silicon dioxide particles) allowed to pass through the filter element is 100nm~600nm.

[0033] During the above treatment process, the pH of the first filtrate f is adjusted to 6-10, for example, the pH is adjusted to 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, 10 or any two thereof. It is generally preferred to adjust the pH to about 8 before performing crystallization treatment.

[0034] Generally, a pH adjusting agent g is used to adjust the pH of the first filtrate f. The pH adjusting agent g can specifically include an alkali, that is, an alkali can be used to adjust the pH of the first filtrate f. Specifically, an alkali can be added to the first filtrate f to adjust the pH of the first filtrate f to 6 to 10. The alkali used can include a soluble alkali, generally an inorganic alkali, such as an alkali metal hydroxide, preferably potassium hydroxide and / or sodium hydroxide.

[0035] In specific implementation, an aqueous solution of pH regulator g (such as alkali solution) can be added to the first filtrate f. The amount of the aqueous solution of pH regulator g added is sufficient to make the pH of the first filtrate f be 6-10, so as to adjust the pH of the first filtrate f to 6-10.

[0036] In some embodiments, the above-mentioned crystallization treatment can be carried out at a temperature of 5°C to 40°C, that is, the temperature of the crystallization treatment can be 5°C to 40°C, for example, 5°C, 10°C, 15°C, 20°C, 25°C, 30°C, 35°C, 40°C or a range composed of any two of them, generally preferably 15°C to 30°C.

[0037] In addition, the crystallization treatment time can generally be 30 to 60 minutes, for example, 30 minutes, 35 minutes, 40 minutes, 45 minutes, 50 minutes, 55 minutes, 60 minutes or any two thereof.

[0038] In addition, if Figure 1 As shown, during the above crystallization treatment, a second agitator can be used for stirring. The second agitator can specifically include a paddle agitator and / or an anchor agitator. The stirring is performed for a preset time (i.e., crystallization treatment time), such as 30 to 60 minutes, and then a second solid-liquid separation is performed.

[0039] When implementing it specifically, Figure 1 As shown, the above-mentioned crystallization treatment can be carried out in a crystallizer 3 with a temperature control system, that is, the first filtrate f enters the crystallizer 3, and then an appropriate amount of alkali solution is added thereto to adjust the pH of the first filtrate f to 6 to 10, for example, the pH of the first filtrate f is adjusted to neutral, and the second agitator is turned on for sufficient stirring (such as stirring for 30 to 60 minutes). If crystallization is carried out at a lower crystallization temperature and cooling is required, the temperature control system (cooling system) of the crystallizer 3 is turned on at the same time to cool the first filtrate f to the crystallization temperature, and crystallization is carried out at the crystallization temperature. After the crystallization is completed, a second solid-liquid separation is carried out to obtain a second solid phase product i and a second filtrate j, respectively.

[0040] Wherein, the second solid phase product i is a crystal precipitated during the crystallization process, mainly including a crystalline salt. In the above-mentioned crystallization process, the anions and cations in the first filtrate f form salt precipitation to form a crystalline salt, wherein the anions, for example, include anions introduced by the acid (catalyst) used during the hydrolysis reaction, and the cations, for example, include cations introduced by the alkali used when adjusting the pH of the first filtrate f. Exemplarily, the alkali used is sodium hydroxide, and the crystalline salt formed by the above-mentioned crystallization process includes a sodium salt. Thus, by the above-mentioned crystallization process, the anions and cations in the filtrate can be removed, and the crystalline salt formed is a harmless solid product, safe and environmentally friendly, and reduces environmental pressure.

[0041] In addition, if Figure 1As shown, a second filter 5 can be used to filter the system after the crystallization treatment (crystallization mixture h) (i.e., second solid-liquid separation), that is, the system after the crystallization treatment enters the second filter 5 for filtration to obtain a second solid phase product i and a second filtrate j, respectively. In the embodiment of the present invention, a conventional filter in the art can be used as the above-mentioned second filter 5, and there is no particular limitation on this.

[0042] The second filtrate j contains an organic phase k and an aqueous phase n. The organic phase k and the aqueous phase n are separated by distillation (or rectification) of the second filtrate j. Figure 1 As shown, a distillation tower 6 (or a distillation separation tower) can be used to distill the second filtrate j. That is, the second filtrate j enters the distillation separation tower for distillation to separate the organic phase k and the aqueous phase n. Usually, the second filtrate j can enter the distillation separation tower from the material inlet in the middle of the distillation separation tower. After distillation, the organic phase k is discharged from the organic phase k outlet at the top of the distillation separation tower, and the aqueous phase n is discharged from the aqueous phase n outlet of the distillation separation tower kettle (generally located at the bottom of the distillation separation tower).

[0043] Generally, the resulting aqueous phase n is water and can be returned to the hydrolysis reaction (i.e., returned to the aforementioned hydrolysis reactor 1) for recycling. The organic phase k comprises an organic alcohol and may also contain a small amount of water. The mass percentage of water in the organic phase k (i.e., the water content of the organic phase k) can be 0.01% to 0.1%, for example, 0.01%, 0.02%, 0.05%, 0.08%, 0.1%, or any combination thereof. The organic phase k can be returned to the silicate production system to continue serving as a raw material for synthesizing silicate.

[0044] Figure 1 The schematic diagram of the structure of the high boiling point processing device of the embodiment of the present invention is shown in FIG. The high boiling point processing device of the embodiment of the present invention can be used to process the high boiling point a, such as Figure 1 As shown, the high-boiling-material treatment device includes a hydrolysis reactor 1 , a first filter 2 , a crystallizer 3 , a second filter 5 and a distillation tower 6 .

[0045] Specifically, the hydrolysis reactor 1 includes a raw material inlet and a first material outlet. The raw material for the hydrolysis reaction (such as the above-mentioned high-boiling substance a, etc.) enters the hydrolysis reactor 1 from the raw material inlet of the hydrolysis reactor 1, and a hydrolysis reaction occurs in the hydrolysis reactor 1. The mixed system after hydrolysis (hydrolyzed mixture d) is discharged from the hydrolysis reactor 1 from the first material outlet.

[0046] Wherein, the feed inlet can comprise the high boiling-material inlet, high boiling-material a enters the hydrolysis reactor 1 from this high boiling-material inlet, catalyzer (as above-mentioned acid) c and other materials such as water b also can enter the hydrolysis reactor 1 (now high boiling-material a and catalyzer c and other materials such as water b enter the hydrolysis reactor 1 by the same inlet) by this high boiling-material inlet, but is not limited to this, the feed inlet can also comprise catalyst inlet and water body inlet, catalyst inlet and water body inlet can be the same inlet, now catalyzer c and water b enter the hydrolysis reactor 1 by this same inlet, for example the aqueous solution of acid enters the hydrolysis reactor 1 by this same inlet, perhaps, catalyst inlet and water body inlet are respectively different inlets, promptly catalyst inlet and water body inlet are respectively set at the different positions of hydrolysis reactor 1, catalyzer c enters the hydrolysis reactor 1 from the catalyst inlet, and water b enters the reactor from the water body inlet.

[0047] For example, Figure 1 As shown, the high-boiling material inlet and the water inlet of the hydrolysis reactor 1 are arranged at the top of the hydrolysis reactor 1, the catalyst inlet is arranged at the upper or middle part of the hydrolysis reactor 1, and the first material outlet is arranged at the bottom of the hydrolysis reactor 1. In this way, the flow of materials in the hydrolysis reactor 1 is facilitated, which is conducive to the progress of the hydrolysis reaction.

[0048] Specifically, if Figure 1 As shown, the hydrolysis reactor 1 includes a first shell 11 and a first cavity 10 enclosed by the first shell 11. The above-mentioned hydrolysis reaction is carried out in the first cavity 10, that is, the first cavity 10 is connected to the above-mentioned raw material inlet, and high-boiling substance a, catalyst c, water b and other materials enter the first cavity 10 for hydrolysis reaction.

[0049] In addition, if Figure 1 As shown, the high-boiling-point processing device further includes a first stirrer provided on the hydrolysis reactor 1 for stirring the system in the hydrolysis reactor 1 so that the hydrolysis reaction proceeds in a stirring state.

[0050] For example, Figure 1 As shown, the first agitator includes a first stirring rod 102 and a first stirring part 101 that are connected to each other. The first stirring rod 102 passes through the first shell 11 and extends into the first cavity 10. The first stirring rod 102 has two opposite ends, one end of which is located outside the first cavity 10, and the other end is located inside the first cavity 10. The end of the first stirring rod 102 located outside the first cavity 10 is connected to a first motor 103 that drives the first stirring part 101 for stirring. The first stirring part 101 is installed at the end of the first stirring rod 102 located in the first cavity 10, that is, the first stirring part 101 is located in the first cavity 10, and when the hydrolysis reaction is carried out, the first stirring part 101 extends into the reaction system to stir the reaction system so that the system undergoes a hydrolysis reaction under stirring.

[0051] Alternatively, as Figure 1 As shown, the first stirring rod 102 is installed at the top of the hydrolysis reactor 1, that is, the first stirring rod 102 passes through the first shell 11 part at the top of the hydrolysis reactor 1, and specifically can pass through the first shell 11 from the middle position of the top first shell 11 part. The water inlet and the high boiling point inlet can be respectively located on opposite sides of the first stirring rod 102.

[0052] As mentioned above, the first stirrer may comprise a paddle stirrer and / or an anchor stirrer, preferably a paddle stirrer.

[0053] The first filter 2 is used to filter the system after the hydrolysis reaction (ie, the hydrolysis mixture d) (ie, perform the first solid-liquid separation) to obtain a first solid phase product e and a first filtrate f, respectively.

[0054] Specifically, the first filter 2 may include a first material inlet, a first filtrate outlet, and a first solid-phase product outlet. The first material inlet is connected to the first material outlet of the hydrolysis reactor 1. Thus, after the high-boiling substance a undergoes a hydrolysis reaction in the hydrolysis reactor 1, the resulting hydrolyzed mixture d is discharged from the first material outlet of the hydrolysis reactor 1 and enters the first filter 2 through the first material inlet for filtration, thereby obtaining a first solid-phase product e and a first filtrate f, respectively. The first solid-phase product e is discharged from the first solid-phase product outlet of the first filter 2, and the first filtrate f is discharged from the first filtrate outlet of the first filter 2 and then enters the crystallizer 3 for crystallization.

[0055] The crystallizer 3 is used to crystallize the first filtrate f from the first filter 2, such as Figure 1 As shown, the crystallizer 3 includes a first filtrate inlet, a second material outlet and a pH regulator inlet.

[0056] Among them, the first filtrate inlet is connected to the first filtrate outlet of the first filter 2, so that the first filtrate f produced by the first filter 2 is discharged through the first filtrate outlet of the first filter 2, and then enters the crystallizer 3 through the first filtrate inlet of the crystallizer 3; the pH regulator inlet is used to add the pH regulator g (such as the above-mentioned alkali solution) into the crystallizer 3 to adjust the pH of the first filtrate f (such as adjusting its pH to 6-10); after crystallization treatment, the formed crystallized mixture h is discharged from the crystallizer 3 from the second material outlet of the crystallizer 3 and enters the second filter 5 for filtration (i.e., the second solid-liquid separation).

[0057] For example, Figure 1 As shown, the first filtrate inlet can be set at the upper part of the crystallizer 3, the pH regulator inlet can be set at the top of the crystallizer 3, and the second material outlet can be set at the bottom of the crystallizer 3.

[0058] Specifically, if Figure 1 As shown, the crystallizer 3 includes a second shell 31 and a second cavity 30 enclosed by the second shell 31. The above-mentioned crystallization process is carried out in the second cavity 30, that is, the second cavity 30 is connected to the above-mentioned first filtrate inlet, the second material outlet and the pH regulator inlet respectively. The pH regulator g enters the second cavity 30 through the pH regulator inlet to adjust the pH of the first filtrate f entering the second cavity 30 through the first filtrate inlet, and then the crystallization process is carried out.

[0059] In addition, if Figure 1 As shown, the crystallizer 3 further includes a temperature adjustment system to adjust the temperature of the first filtrate f to the above-mentioned crystallization temperature, so that the first filtrate f is crystallized at the crystallization temperature.

[0060] Specifically, if Figure 1 As shown, the temperature control system includes a jacket 4 arranged outside the crystallizer, and a circulating medium for regulating the temperature in the crystallizer exists in the jacket 4.

[0061] like Figure 1 As shown, the jacket 4 includes a side wall 41 arranged around the crystallizer 3 and a bottom wall 42 located at the bottom of the crystallizer 3. The side wall 41 and the bottom wall 42 are connected and enclosed to form a third cavity 40. The crystallizer 3 is located in the third cavity 40.

[0062] Specifically, the jacket 4 can be connected to a temperature control unit, and a circulating medium of a preset temperature is introduced into the jacket 4 through the temperature control unit. The circulating medium of the preset temperature circulates between the jacket and the temperature control unit, and the temperature inside the crystallizer 3 is regulated by the circulating medium of the preset temperature.

[0063] For example, when the crystallization temperature is low or needs to be cooled, the temperature control system can be specifically a cooling system, and the circulating medium is a cooling medium, such as chilled water. The temperature control unit supplies circulating cooling medium to the jacket 4 to cool the system in the crystallizer 3 or maintain its lower crystallization temperature.

[0064] In addition, if Figure 1 As shown, the high-boiling-point processing device may further include a second agitator provided on the crystallizer, for agitating the system in the crystallizer 3 so that the pH regulator and the first filtrate f are fully mixed and the crystallization process is carried out in a stirring state.

[0065] Specifically, if Figure 1As shown, the second agitator includes a second stirring rod 302 and a second stirring part 301 connected to each other. The second stirring rod 302 passes through the second shell 31 and extends into the second cavity 30. The second stirring rod 302 has two opposite ends, one end of which is located outside the second cavity 30, and the other end is located inside the second cavity 30. The end of the second stirring rod 302 located outside the cavity is connected to a second motor 303 that drives the second stirring part 301 for stirring. The second stirring part 301 is installed at the end of the second stirring rod 302 located in the second cavity 30, that is, the second stirring part 301 is located in the second cavity 30. After the first filtrate f enters the crystallizer 3 from the first filtrate inlet of the crystallizer 3, the second stirring part 301 extends into the first filtrate f to stir the first filtrate f.

[0066] For example, Figure 1 As shown, the second stirring rod 302 is arranged at the top part of the second shell 31 (that is, the second shell 31 part arranged at the top of the crystallizer 3), and it passes through the second shell 31 part at the top of the crystallizer 3, specifically, it can pass through the second shell 31 from the middle position of the second shell 31 part at the top.

[0067] As mentioned above, the second stirrer may comprise a paddle stirrer and / or an anchor stirrer, preferably a paddle stirrer.

[0068] The second filter 5 is used to filter the crystallized mixture h from the crystallizer 3 (ie, perform a second solid-liquid separation) to obtain a second solid phase product i and a second filtrate j, respectively.

[0069] Specifically, if Figure 1 As shown, the second filter 5 includes a second material inlet, a second filtrate outlet and a second solid product outlet.

[0070] Among them, the second material inlet is connected to the second material outlet of the crystallizer 3. Thus, after the first filtrate f is crystallized in the crystallizer 3, the formed crystallized mixture h is discharged from the second material outlet of the crystallizer 3 and enters the second filter 5 through the second material inlet of the second filter 5 for filtration to obtain a second solid phase product i and a second filtrate j, respectively; the second solid phase product i is discharged from the second solid phase product outlet of the second filter 5, and the second filtrate j is discharged from the second filtrate outlet of the second filter 5 and enters the distillation tower 6 for distillation.

[0071] like Figure 1As shown, the distillation tower 6 is used to distill the second filtrate j to separate the organic phase k and the aqueous phase n. The distillation tower 6 includes a second filtrate inlet, an organic phase outlet for outputting the organic phase k, a condenser 601, a liquid phase inlet, a water phase outlet for outputting the water phase n, a reboiler 602 and a gas phase inlet. The second filtrate inlet is connected to the second filtrate outlet of the second filter 5, the organic phase outlet, the condenser 601, and the liquid phase inlet are connected in sequence, and the water phase outlet, the reboiler 602, and the gas phase inlet are connected in sequence.

[0072] Thus, the second filtrate j produced by the second filter 5 is discharged from the second filtrate outlet of the second filter 5, enters the distillation tower 6 through the second filtrate inlet of the distillation tower 6, and is distilled in the second distillation tower 6. The generated organic phase k is discharged from the distillation tower 6 through the organic phase outlet, part of the organic phase k is output as the product, and part is condensed through the condenser 601 (generally, the organic phase k is liquefied) and returned to the distillation tower 6 from the liquid phase inlet to form a cycle. The generated water phase n is discharged from the distillation tower 6 through the water phase outlet of the distillation tower 6, part of it is vaporized through the reboiler 602 and returned to the distillation tower 6 from the gas phase inlet to form a cycle, and part of it can return to the hydrolysis reactor to participate in the hydrolysis reaction.

[0073] For example, Figure 1 As shown, the second filtrate inlet of the distillation tower 6 is arranged in the middle of the distillation tower 6, the organic phase outlet can be arranged at the upper part of the distillation tower 6, the liquid phase inlet can be arranged at the top of the distillation tower 6, the water phase outlet is arranged at the bottom of the distillation tower 6, and the gas phase inlet is arranged at the lower part of the distillation tower 6.

[0074] Specifically, the distillation tower 6 includes a distillation section and a tower kettle which are interconnected. The tower kettle is located at the lower part of the distillation section. The second filtrate inlet of the distillation tower 6 is connected to the distillation section. The organic phase outlet and the liquid phase inlet are arranged on the distillation section. The organic phase outlet can be specifically arranged at the upper part of the distillation section (also the upper part of the distillation tower 6), and the liquid phase inlet can be specifically arranged at the top of the distillation section (also the top of the distillation tower 6). The water phase outlet and the gas phase inlet are arranged on the tower kettle. The water phase outlet can be specifically arranged at the bottom of the tower kettle (also the bottom of the distillation tower 6), and the gas phase inlet can be specifically arranged at the upper, middle or lower part of the tower kettle.

[0075] Among them, the filtrate from the second filter 5 enters the distillation section of the distillation tower 6 from the second filtrate inlet of the distillation tower 6, and is distilled in the distillation section. The generated organic phase k is discharged from the organic phase outlet provided in the distillation section. Part of it is used as the product, and part of it is condensed through the condenser 601 and returned to the distillation section from the liquid phase inlet. The water phase n enters the tower kettle and is discharged through the water phase outlet provided in the tower kettle. Part of it is vaporized through the reboiler 602 and returned to the tower kettle from the gas phase inlet to form a cycle. Part of it can return to the hydrolysis reactor 1 to participate in the hydrolysis reaction.

[0076] Specifically, the distillation separation tower may include a plate tower and / or a packed tower, and a packed tower is generally preferred, but not limited thereto.

[0077] In general, if Figure 1 As shown, the hydrolysis reactor 1, the crystallizer 3, and the distillation tower 6 can be placed vertically, and the axial / length direction of the hydrolysis reactor 1, the direction from the bottom to the top of the hydrolysis reactor 1, the axial / length direction of the crystallizer 3, the direction from the bottom to the top of the crystallizer 3, the axial / length direction of the distillation tower 6, and the direction from the bottom to the top of the distillation tower 6 are basically parallel to each other.

[0078] The hydrolysis reactor 1, the first filter 2, the crystallizer 3, the second filter 5, the distillation tower 6, the condenser 601, the reboiler 602, etc. can be conventional equipment or components with corresponding functions in the art, and there is no particular limitation on this.

[0079] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the above embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for treating high boiling substances, characterized in that: The high boiling substances include high boiling substances discharged from the silicate production process, and the high boiling substance treatment method includes: The high boiling point product is subjected to a hydrolysis reaction under the action of a catalyst, and then subjected to a first solid-liquid separation to obtain a first solid phase product and a first filtrate, respectively; wherein the catalyst comprises an acid; adjusting the pH of the first filtrate to 6-10, and sequentially performing crystallization treatment and second solid-liquid separation to obtain a second solid phase product and a second filtrate, respectively; distilling the second filtrate using a distillation tower to obtain an organic phase and an aqueous phase; Returning at least a portion of the aqueous phase to participate in the hydrolysis reaction, and returning a portion of the aqueous phase to the distillation tower through the gas phase inlet after being vaporized in the distillation tower; The high boilers include polysilicates and organic alcohols.

2. The high boiling point treatment method according to claim 1, wherein The acid includes inorganic acids.

3. The high boiling point treatment method according to claim 2, wherein: The inorganic acid includes hydrochloric acid and / or sulfuric acid.

4. The high boiling point treatment method according to claim 1, wherein The hydrolysis reaction time is 30 minutes to 120 minutes; and / or, During the hydrolysis reaction, a first stirrer is used for stirring, and the first stirrer includes a paddle stirrer and / or an anchor stirrer.

5. The high boiling point treatment method according to claim 1, wherein Performing the first solid-liquid separation by filtration with a filtration accuracy of 100 nm to 600 nm to obtain the first solid phase product and the first filtrate; And / or, the first solid phase product comprises silicon dioxide.

6. The high boiling point treatment method according to claim 1, wherein: Adding a base to the first filtrate to adjust the pH of the first filtrate to 6-10, wherein the base includes potassium hydroxide and / or sodium hydroxide.

7. The high boiling point treatment method according to claim 1, wherein: The crystallization treatment is carried out at a temperature of 5°C to 40°C.

8. The high boiling point treatment method according to claim 1 or 7, characterized in that: During the crystallization treatment, a second stirrer is used for stirring, wherein the second stirrer includes a paddle stirrer and / or an anchor stirrer, and the stirring time is 30 minutes to 60 minutes.

9. The high boiling point treatment method according to claim 1, wherein: The organic phase includes an organic alcohol; And / or, the mass percentage of water in the organic phase is 0.01% to 0.1%.

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