A system and method for separating 1,5-pentanediamine
Through the combination of the steam generation device and the refining device, the temperature control treatment under conveyor belt heating and vacuum conditions are used to solve the problem of impurities in the aqueous phase affecting the distillation efficiency, and the continuous separation and efficient treatment of high-purity 1,5-pentanediamine are achieved.
Patent Information
- Application Number
- CN202110417125.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2021-04-19
- Publication Date
- 2025-07-11
- Estimated Expiration
- 2041-04-19
AI Technical Summary
In the prior art, when 1,5-pentanediamine is produced in biological methods, impurities in the aqueous phase lead to a decrease in distillation efficiency, making it difficult to efficiently separate high-purity 1,5-pentanediamine.
The steam generation device and the refining device are used to evaporate 1,5-pentanediamine into a gaseous state through the conveyor belt heating treatment, the heating temperature is controlled by vacuum conditions and temperature control components, and the condensation device is combined to achieve continuous separation and refining, and the treatment is performed using a vacuum belt dryer.
The continuous separation of high-purity 1,5-pentanediamine is achieved, which improves separation efficiency, reduces the equipment footprint and operating power, and simplifies the operation process.
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Figure CN115212597B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to 1,5 - diamino - pentane, and particularly to a system and method for separating 1,5 - diamino - pentane. Background Art
[0002] 1,5 - Diamino - pentane (Diaminopentane; DN5, hereinafter referred to as pentamethylenediamine), also known as cadaverine, has a wide range of applications in agriculture, medicine, and industry. The conventional extraction method of 1,5 - diamino - pentane produced by biological methods requires separating 1,5 - diamino - pentane from the aqueous phase. Since the aqueous phase also contains sugars, proteins, metabolic by - products, and inorganic salt impurities brought about by the biological conversion process, if conventional distillation is used to extract 1,5 - diamino - pentane, the viscosity of the system will increase in the later stage of distillation, resulting in a reduction in distillation efficiency. Summary of the Invention
[0003] The present invention provides a system for separating 1,5 - diamino - pentane, including a vapor generation device and a refining device; wherein, the vapor generation device is used to heat - treat a raw material liquid containing 1,5 - diamino - pentane to obtain a vapor containing 1,5 - diamino - pentane; the refining device is used to refine the liquid obtained after condensing the vapor containing 1,5 - diamino - pentane to obtain 1,5 - diamino - pentane; the vapor generation device includes a conveyor belt, a driving component, and a temperature - control component; the conveyor belt is used to carry the raw material liquid, the temperature - control component is used to heat - treat the raw material liquid on the conveyor belt, and the driving component is used to drive the conveyor belt to rotate in a cycle.
[0004] An embodiment of the present invention further provides a method for separating 1,5 - diamino - pentane, including:
[0005] Heat - treating a raw material liquid containing 1,5 - diamino - pentane through a vapor generation device to obtain a vapor containing 1,5 - diamino - pentane; and
[0006] Refining the liquid obtained after condensing the vapor containing 1,5 - diamino - pentane to obtain a 1,5 - diamino - pentane product;
[0007] Wherein, the vapor generation device includes a conveyor belt, a driving component, and a temperature - control component; the conveyor belt is used to carry the raw material liquid, the temperature - control component is used to heat - treat the raw material liquid on the conveyor belt, and the driving component is used to drive the conveyor belt to rotate in a cycle.
[0008] An embodiment of the present invention further provides a 1,5 - diamino - pentane product prepared by the above - mentioned method.
[0009] An embodiment of the present invention further provides an application of a belt dryer, especially a vacuum belt dryer, in separating 1,5 - diamino - pentane.
[0010] The system for separating 1,5-pentanediamine according to an embodiment of the present invention has a high degree of equipment automation and a high material processing load, can obtain a 1,5-pentanediamine product with high purity, and realizes the continuous separation of 1,5-pentanediamine. Brief Description of the Drawings
[0011] Figure 1 It is a schematic structural diagram of the system for separating 1,5-pentanediamine according to an embodiment of the present invention. Detailed Embodiments
[0012] Typical embodiments embodying the features and advantages of the present invention will be described in detail in the following description. It should be understood that the present invention can have various changes in different embodiments, all of which do not depart from the scope of the present invention, and the descriptions and illustrations therein are for illustrative purposes in nature and are not intended to limit the present invention.
[0013] As Figure 1 shown, an embodiment of the present invention provides a system for separating 1,5-pentanediamine, including:
[0014] A vapor generation device for obtaining a vapor containing 1,5-pentanediamine by heating a raw material liquid containing 1,5-pentanediamine; and
[0015] A refining device for refining the liquid obtained after condensing the above-mentioned vapor to obtain 1,5-pentanediamine;
[0016] Wherein, the vapor generation device includes a conveyor belt 11, a driving component, and a temperature control component; the conveyor belt 11 is used to carry the raw material liquid, the temperature control component is used to heat the raw material liquid on the conveyor belt 11, and the driving component is used to drive the conveyor belt 11 to rotate in a cycle.
[0017] According to some embodiments of the present invention, the refining device includes one or more of a rectification device, a distillation device, and an evaporation device.
[0018] In one embodiment, the temperature control component includes a first temperature control component 13, and the first temperature control component 13 acts on the conveyor belt 11 to heat the raw material liquid located on the conveyor belt 11.
[0019] A system for separating 1,5-pentanediamine according to an embodiment of the present invention. During operation, after the raw material liquid on the conveyor belt 11 is heated by the first temperature control component 13, 1,5-pentanediamine and water in it evaporate into gas state, and the remaining residue can fall off automatically at the winding end of the annular conveyor belt 11. At the same time, with the reciprocating rotation of the conveyor belt 11, the raw material liquid can be continuously set on the conveyor belt 11 for heating treatment, continuously obtaining the vapor containing 1,5-pentanediamine, and continuously refining this vapor through the refining device to obtain 1,5-pentanediamine product, realizing the continuous separation of 1,5-pentanediamine.
[0020] In one embodiment, the driving component includes a first roller 12a, a second roller 12b and a power source, and the power source can be a motor for example. Wherein, the conveyor belt 11 is sleeved on the first roller 12a and the second roller 12b.
[0021] In one embodiment, the temperature control component is located between the first roller 12a and the second roller 12b.
[0022] In one embodiment, the vapor generating device includes a cloth-feeding component 10 to set the raw material liquid on the conveyor belt 11. For example, the raw material liquid can be cloth-fed on the conveyor belt 11 in the form of a thin layer through the cloth-feeding component 10.
[0023] In one embodiment, the cloth-feeding component 10 can be a cloth-feeding pipe.
[0024] In one embodiment, the cloth-feeding component 10 is arranged adjacent to the first roller 12a and is located above the conveyor belt 11.
[0025] In one embodiment, the temperature control component includes a first temperature control component 13 and a second temperature control component 14. The first temperature control component 13 is used to perform the first heating treatment on the raw material liquid to form the vapor containing 1,5-pentanediamine and the residue remaining on the conveyor belt 11; the second temperature control component 14 is used to perform the second heating treatment on the remaining residue.
[0026] In one embodiment, the first temperature control component 13 and the second temperature control component 14 act on the conveyor belt 11 to heat the raw material liquid and / or the remaining residue located on the conveyor belt 11.
[0027] In one embodiment, the conveyor belt 11 includes a first surface and a second surface oppositely arranged to the first surface. The first surface is used to carry the raw material liquid, and the cloth-feeding component 10 can be located above the first surface; the first temperature control component 13 and the second temperature control component 14 act on the second surface of the conveyor belt 11, that is, the first temperature control component 13 and the second temperature control component 14 are located below the conveyor belt 11.
[0028] In one embodiment, the number of the first temperature control component 13 and the second temperature control component 14 can be one or more respectively, for example, 2, 3, 4, 6 or 7.
[0029] In one embodiment, both the first temperature control component 13 and the second temperature control component 14 can be metal heating plates.
[0030] In one embodiment, the heating methods of the metal heating plates include one or more of steam heating, heat transfer oil heating, and electric heating.
[0031] In one embodiment, the conveyor belt 11 is a crawler belt.
[0032] In one embodiment, the material of the conveyor belt 11 can be a fiberglass reinforced material with a Teflon coating, etc.
[0033] In one embodiment, the number of the conveyor belts 11 can be one layer or multiple layers, for example, 3 to 13 layers.
[0034] In one embodiment, both the first temperature control component 13 and / or the second temperature control component 14 can be slidably attached to the second surface of the conveyor belt 11, that is, the positions of the first temperature control component 13 and the second temperature control component 14 will not change with the cyclic rotation of the conveyor belt 11.
[0035] In one embodiment, along the transmission direction of the conveyor belt 11, the first temperature control component 13 and the second temperature control component 14 are located between the first roller 12a and the second roller 12b.
[0036] In one embodiment, the first temperature control component 13 is adjacent to the first roller 12a, the second temperature control component 14 is adjacent to the second roller 12b, and the remaining residues on the conveyor belt 11 can fall off the conveyor belt 11 through the winding end of the second roller 12b.
[0037] In one embodiment, the vapor generating device includes a collecting device 16, and the residues falling off the conveyor belt 11 can directly enter the collecting device 16.
[0038] In one embodiment, the vapor generating device can include a crushing component 15. The large residues on the conveyor belt 11 can be crushed by the crushing component 15, and the crushed residues can enter the collecting device 16.
[0039] In one embodiment, the crushing component 15 can be arranged outside the second roller 12b, that is, along the transmission direction of the conveyor belt 11, the crushing component 15 is arranged on the side far from the first roller 12a.
[0040] In one embodiment, the crushing component 15 can be, for example, an auger, a toothed crushing device, etc.
[0041] In one embodiment, the vapor generating device may include a scraper (not shown in the figure), which acts on the first surface of the conveyor belt 11 to scrape off the residues on the first surface of the conveyor belt 11, so as to reduce the residue of solid slag on the first surface, facilitating the subsequent cyclic operation of "feeding → evaporation → slag removal".
[0042] In one embodiment, the scraper acts on the first surface of the conveyor belt 11 and is close to the second roller 12b.
[0043] In one embodiment, the collecting device 16 may be, for example, a storage tank or a conveying trough with a crushing function.
[0044] In one embodiment, the collecting device 16 is a conveying trough with a crushing function. In the collecting device 16, the residues are crushed into appropriate particle sizes and then conveyed out of the vapor generating device.
[0045] In one embodiment, the collecting device 16 is adjacent to the second roller 12b and may be located below the second roller 12b, so that the residues (or the crushed residues) falling off from the winding end of the second roller 12b can directly fall into the collecting device 16.
[0046] In one embodiment, the vapor generating device includes a housing with an accommodating space, and the conveyor belt 11, the driving component, the temperature control component, the crushing component 15, and the collecting device 16 are all located inside the housing.
[0047] In one embodiment, the vapor generating device includes a heat insulation layer 17, which is arranged on the housing so that the vapor containing 1,5-pentanediamine can maintain a gaseous state inside the housing, and the yield of 1,5-pentanediamine can be further improved.
[0048] In one embodiment, the heat insulation layer 17 may be, for example, a steam jacket layer, a circulating water jacket layer, or a heat transfer oil jacket layer.
[0049] In one embodiment, the heat insulation layer 17 contains a heating component, such as an electric heating component.
[0050] In one embodiment, the heat insulation layer 17 can be arranged inside the housing or outside the housing.
[0051] In one embodiment, the vapor generating device includes a vacuum component 18, which can perform a pressure reduction treatment on the space inside the housing to obtain the required vacuum environment.
[0052] In one embodiment, the vacuum component 18 can be arranged outside the housing of the vapor generating device, and it can be a vacuum pump.
[0053] In one embodiment, the vapor generating device is connected to a refining device 20, and the refining device 20 may be, for example, a distillation column.
[0054] In one embodiment, the system for separating 1,5-pentanediamine includes a condensation device 30, which is respectively connected to a vapor generation device and a refining device 20 to condense the vapor containing 1,5-pentanediamine into a liquid and then perform refining treatment.
[0055] In one embodiment, when the condensation device 30 is connected to the steam generation device, the position of the condensation device 30 should be as convenient as possible for collecting the vapor containing 1,5-pentanediamine. For example, since the generated 1,5-pentanediamine vapor is easy to accumulate in the upper half of the cavity of the steam generation device due to its low density, preferably, the condensation device 30 is connected to the upper half of the outer shell of the steam generation device.
[0056] In one embodiment, the condensation device 30 can be a heat exchanger.
[0057] In one embodiment, the vacuum component 18 is connected to the inside of the outer shell of the vapor generation device through the condensation device 30.
[0058] In one embodiment, the system for separating 1,5-pentanediamine includes a feed tank 40, in which a solution system containing 1,5-pentanediamine salt can be alkalized to form a raw material liquid containing 1,5-pentanediamine; wherein, the alkalization treatment refers to the reaction of salt with alkali.
[0059] In one embodiment, the feed tank 40 includes a stirring component and / or a third temperature control component, and the raw material liquid can be preheated through the third temperature control component.
[0060] In one embodiment, the system for separating 1,5-pentanediamine includes a feed pump 50, and the feed pump 50 is respectively connected to the feed tank 40 and the cloth-feeding component 10 of the vapor generation device to transport the raw material liquid to the cloth-feeding component 10.
[0061] In one embodiment, the system for separating 1,5-pentanediamine includes a concentration tank (not shown in the figure), and the concentration tank can be located upstream of the feed tank 40, that is, the concentration tank, the feed tank 40, and the vapor generation device are connected in sequence.
[0062] In one embodiment, the vapor generation device can be a belt dryer, and further can be a vacuum belt dryer. Among them, the foregoing limitations on the structure of the vapor generation device are all applicable to the belt dryer.
[0063] In one embodiment, the belt dryer can be an existing device.
[0064] In one embodiment, the raw material liquid is a solution system containing 1,5-pentanediamine.
[0065] In one embodiment, the raw material liquid contains 1,5-pentanediamine and water.
[0066] In one embodiment, the mass content of 1,5-pentanediamine in the raw material liquid is 8% to 75%, such as 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, etc.
[0067] In one embodiment, the raw material liquid contains an alkali metal salt, and the mass of the alkali metal salt accounts for 30 to 80% of the mass of the solids in the raw material liquid, further 40 to 60%. The alkali metal mainly comes from the alkaline substances used in the process of preparing the 1,5-pentanediamine alkalization liquid.
[0068] In one embodiment, the mass content (solid content) of the solids in the raw material liquid is 10 to 80%, further 20 to 70%, such as 30%, 40%, 50%, etc.
[0069] The solid content refers to the mass content of the residue remaining after the raw material liquid is treated by the steam generating device in the raw material liquid.
[0070] In one embodiment, the density of the raw material liquid is 1.02 to 1.25 g / cm 3 。
[0071] In one embodiment, the pH of the raw material liquid > 12.3.
[0072] In one embodiment, the raw material liquid is an alkalization liquid containing 1,5-pentanediamine.
[0073] In one embodiment, the preparation process of the alkalization liquid containing 1,5-pentanediamine includes: adding an alkaline substance (alkaline treatment) to the solution system containing 1,5-pentanediamine salt, wherein the 1,5-pentanediamine salt reacts with the alkaline substance to generate 1,5-pentanediamine, thereby forming a solution system containing free 1,5-pentanediamine (alkalization liquid containing 1,5-pentanediamine).
[0074] In one embodiment, concentration treatment can be carried out before or after the alkalization treatment of the solution system containing 1,5-pentanediamine salt.
[0075] In one embodiment, the alkaline substance may include but is not limited to one or more of alkali metal oxides / hydroxides, alkaline earth metal oxides / hydroxides, and corresponding alkaline salts (such as sodium phosphate, potassium phosphate, sodium carbonate, potassium carbonate, etc.).
[0076] In one embodiment, the method of adding an alkaline substance to a solution system containing 1,5-pentanediamine salt can be a one-time addition or multiple additions. If multiple bases are added, they can be first mixed into a base mixture and then added, or each base can be added separately. The base mixture can include one or more strong bases and one or more weak bases. Alkaline substances include, but are not limited to, calcium oxide, calcium hydroxide, magnesium oxide, magnesium hydroxide, sodium phosphate, sodium carbonate, sodium hydroxide, potassium hydroxide, and their combinations. The base can be added in the form of a solid and / or a solution (such as an aqueous solution). The amount of the base used is such that the 1,5-pentanediamine salt in the solution system containing 1,5-pentanediamine salt can be substantially completely converted into 1,5-pentanediamine. The base can be added to the solution system containing 1,5-pentanediamine salt at any suitable temperature as long as the 1,5-pentanediamine salt can be converted into 1,5-pentanediamine at this temperature.
[0077] In one embodiment, the solution system containing 1,5-pentanediamine salt includes a fermentation broth or an enzyme conversion broth containing 1,5-pentanediamine salt.
[0078] The present invention does not particularly limit the specific preparation method of the enzyme conversion broth containing 1,5-pentanediamine salt or directly fermenting to prepare 1,5-pentanediamine. Those of ordinary skill in the art can select specific raw materials according to the prior art and determine the process parameters of the specific enzyme conversion process, thereby obtaining an aqueous solution containing 1,5-pentanediamine salt.
[0079] In one embodiment, the solution system containing 1,5-pentanediamine salt is an enzyme conversion broth of 1,5-pentanediamine salt, which can be obtained by reacting a lysine salt solution under the action of lysine decarboxylase (LDC). Among them, the lysine salt can be an inorganic salt or an organic salt of lysine, such as commercially available lysine hydrochloride, lysine sulfate, etc.
[0080] In one embodiment, the solution system containing 1,5-pentanediamine salt is a fermentation broth of 1,5-pentanediamine salt, which can be obtained by the following method: Through genetic technology, upregulating the expression of lysine decarboxylase in a strain capable of producing lysine, or recombinantly expressing lysine decarboxylase, can synchronously convert the produced lysine into pentanediamine during the fermentation process, thereby directly obtaining a fermentation broth containing 1,5-pentanediamine salt. The present invention has no particular requirements for the recombinant bacteria as long as 1,5-pentanediamine can be obtained.
[0081] One embodiment of the present invention provides a method for separating 1,5-pentanediamine, including:
[0082] heating a raw material liquid containing 1,5-pentanediamine through a steam generating device to obtain a steam containing 1,5-pentanediamine; and
[0083] The liquid obtained by condensing the above-mentioned vapor is refined to obtain 1,5-pentanediamine;
[0084] Among them, the structure of the vapor generation device is applicable to the aforementioned limitations.
[0085] According to some embodiments of the present invention, the refining treatment includes one or more of rectification, distillation, and evaporation.
[0086] The method for separating 1,5-pentanediamine according to an embodiment of the present invention can be completed by the aforementioned system for separating 1,5-pentanediamine.
[0087] In one embodiment, the vapor generation device is a belt dryer, and further a vacuum belt dryer. Among them, the belt dryer can be an existing device.
[0088] The method according to an embodiment of the present invention includes preheating the raw material liquid to a certain temperature and then introducing it into the vapor generation device.
[0089] In one embodiment, the feeding temperature of the raw material liquid into the vapor generation device is 40-130 °C, such as 55 °C, 60 °C, 65 °C, 70 °C, 75 °C, 80 °C, 85 °C, 90 °C, 95 °C, 100 °C, 110 °C, 115 °C, 120 °C, 125 °C, etc.
[0090] In one embodiment, the raw material liquid is arranged in a thin layer on the conveyor belt 11 and then subjected to heat treatment.
[0091] In one embodiment, methods such as reciprocating spraying and / or thin-layer coating can be used for feeding to form a thin-layer material on the conveyor belt 11.
[0092] In one embodiment, the thickness of the thin layer can be 0.5-30 mm, and further can be 2-20 mm, such as 1 mm, 2 mm, 8 mm, 10 mm, 12 mm, 15 mm, 23 mm, 25 mm, 28 mm, etc.
[0093] In one embodiment, the heat treatment includes a first heat treatment. The raw material liquid containing 1,5-pentanediamine forms a vapor containing 1,5-pentanediamine and a residue containing residues after the first heat treatment. The first heat treatment can be realized by the first temperature control component 13.
[0094] In one embodiment, the heating temperature of the first temperature control component 13 or the first heat treatment can be 105-250 °C, and further can be 135-240 °C, such as 110 °C, 120 °C, 130 °C, 140 °C, 150 °C, 160 °C, 170 °C, 180 °C, 190 °C, 210 °C, 220 °C, 240 °C, 245 °C, etc.
[0095] In one embodiment, the degree of vacuum of the vapor generating device or the first heat treatment is 10 Pa to 10 KPa, further 50 to 3000 Pa, and still further 50 to 1000 Pa, such as 20 Pa, 50 Pa, 80 Pa, 100 Pa, 200 Pa, 500 Pa, 800 Pa, 1 KPa, 2 KPa, 5 KPa, 8 KPa, etc.
[0096] In one embodiment, the vapor containing 1,5-pentanediamine includes 1,5-pentanediamine gas and water vapor.
[0097] In one embodiment, the residence time of the material on the conveyor belt 11 above the first temperature control member 13 or the time of the first heat treatment is 20 to 300 min, further 30 to 120 min, such as 50 mm, 60 mm, 80 mm, 100 mm, 150 mm, 180 mm, 200 mm, 250 mm, etc.
[0098] In one embodiment, the method for separating 1,5-pentanediamine further includes performing a second heat treatment on the residue-containing residue, which can be achieved by the second temperature control member 14. The heating temperature of the second temperature control member 14 or the second heat treatment can be 50 to 180 °C, further 50 to 150 °C, such as 60 °C, 70 °C, 80 °C, 90 °C, 100 °C, 110 °C, 120 °C, 140 °C, 160 °C, 170 °C, etc.
[0099] In one embodiment, the heating temperature of the first heat treatment is greater than the heating temperature of the second heat treatment.
[0100] In one embodiment, laying the material on the surface of the conveyor belt 11 to have a suitable thickness can not only improve the evaporation efficiency but also does not require a high evaporation temperature.
[0101] In one embodiment, the solid content in the raw material liquid containing 1,5-pentanediamine for feeding is relatively low. Under the condition of laying the same thickness, the evaporation speed is relatively fast, and the content of 1,5-pentanediamine remaining in the solid residue will relatively increase.
[0102] In one embodiment, the vapor containing 1,5-pentanediamine is discharged from the vapor generating device. After it is condensed into a liquid, the obtained liquid is subjected to a refining treatment to obtain a 1,5-pentanediamine product.
[0103] In one embodiment, the vapor containing 1,5-pentanediamine discharged from the vapor generating device is subjected to a condensation treatment to condense the vapor into a liquid and then perform a refining treatment; wherein, the condensation treatment can be natural cooling or can be cooling through the condensation device 30.
[0104] In one embodiment, the vapor containing 1,5-pentanediamine is heat-insulated so that it can remain in a gaseous state before the refining process, thereby further improving the yield of 1,5-pentanediamine.
[0105] In one embodiment, after the first heat treatment is completed, the residue remaining on the conveyor belt 11 can flake off by itself at the winding end of the conveyor belt 11, or flake off by itself at the winding end of the conveyor belt 11 after the second heat treatment.
[0106] In one embodiment, the residue remaining on the conveyor belt 11 can be crushed, and then the residue falls off at the winding end of the conveyor belt 11.
[0107] The method according to one embodiment of the present invention includes:
[0108] Adding a solution system containing 1,5-pentanediamine salt (concentrated or not concentrated) and an alkali solution to the feed tank 40, forming a raw material liquid containing free 1,5-pentanediamine through alkalization treatment in the feed tank 40, and preheating it to 50-100 °C;
[0109] Transporting the raw material liquid to the cloth component 10 of the vapor generating device through the feed pump 50, forming a vacuum environment inside the housing of the vapor generating device through the vacuum component 18, and forming a thin-layer material on the conveyor belt 11 through the cloth component 10;
[0110] The conveyor belt 11 contacts the first temperature control component 13 to heat the raw material liquid located thereon under vacuum conditions to generate a gas mixture containing 1,5-pentanediamine and water vapor. This gas mixture is discharged from the vapor generating device under the action of the vacuum component 18 and forms a condensate containing 1,5-pentanediamine through the condensation device 30;
[0111] Obtaining pure pentanediamine by refining the condensate containing 1,5-pentanediamine. The refining process includes but is not limited to rectification, distillation, evaporation, etc.;
[0112] The material remaining on the conveyor belt 11 after being heated by the first temperature control component 13 enters above the second temperature control component 14 as the conveyor belt 11 runs. The conveyor belt 11 contacts the second temperature control component 14 to perform a second heat treatment on the material located thereon; the material after the second heat treatment continues to move with the conveyor belt 11 to the winding end and flakes off by itself, or the large pieces of material are crushed by the reciprocating crushing component 15, and the crushed material then falls into the collection device 16 with a crushing function.
[0113] Since the heating temperature of the second temperature control component 14 is lower than that of the first temperature control component 13, the temperature of the material after being heated by the second temperature control component 14 is lower than the temperature of the material after being heated by the first temperature control component 13.
[0114] In one embodiment, the residual amount of 1,5-pentanediamine in the remaining residue output from the conveyor belt 11 is not higher than 15 wt%, further not higher than 8 wt%, further 0.3 - 8 wt%, and still further 0.5 - 8 wt%.
[0115] In one embodiment, the yield of 1,5-pentanediamine ≥ 90 wt%, further ≥ 95 wt%.
[0116] One embodiment of the present invention provides a 1,5-pentanediamine product prepared by the above method. The purity of the 1,5-pentanediamine product can be above 98.5 wt%, further above 99 wt%, the water content < 1000 ppm, the color number < 10, further < 5, and the content of tetrahydropyridine < 1000 ppm, further < 800 ppm.
[0117] One embodiment of the present invention provides an application of a belt dryer in the separation of 1,5-pentanediamine, and further provides an application of a vacuum belt dryer in the separation of 1,5-pentanediamine.
[0118] One embodiment of the present invention provides a method for separating 1,5-pentanediamine, which includes treating a raw material liquid containing 1,5-pentanediamine with a belt dryer, preferably a vacuum belt dryer.
[0119] Among them, the above description of the method for separating 1,5-pentanediamine is equally applicable to the use of the aforementioned system for separating 1,5-pentanediamine.
[0120] The system for separating 1,5-pentanediamine according to one embodiment of the present invention has a small equipment operation power, a small floor area, a high degree of automation, and a high material handling load for the equipment. It can handle complex materials and can obtain a 1,5-pentanediamine product with high purity, realizing the continuous separation of 1,5-pentanediamine.
[0121] The method for separating 1,5-pentanediamine according to one embodiment of the present invention has a simple process and a high degree of automation. It can obtain a 1,5-pentanediamine product with high purity, realizing the continuous separation of 1,5-pentanediamine. The residue is easy to handle.
[0122] The system / method for separating 1,5-pentanediamine according to one embodiment of the present invention can overcome the problem of difficult distillation caused by the bottom residue in the later stage of distillation (after alkalization) in the traditional separation device / method, thereby making the yield of 1,5-pentanediamine unsatisfactory.
[0123] Hereinafter, the system and method for separating 1,5-pentanediamine according to one embodiment of the present invention will be further described in combination with specific examples and drawings. Among them, the raw materials used, unless otherwise specified, are all obtained commercially, and the test methods adopted are as follows:
[0124] Detection method for pentanediamine purity and tetrahydropyridine content: detected by gas phase normalization method.
[0125] Color number: platinum-cobalt standard colorimetric method.
[0126] Example 1
[0127] Preheat the alkalized solution containing 1,5-pentanediamine in the feed tank 40 (the solid content of the alkalized solution is 35%, the mass concentration of 1,5-pentanediamine in the alkalized solution is 60%, the density of the alkalized solution is 1.18, the pH of the alkalized solution is 12.8, and the proportion of alkali metal salts in the solid matter in the alkalized solution is 50%) to 100 °C; pass the preheated raw material liquid into the cloth component 10 through the feed pump 50, and continuously spread the raw material liquid on the conveyor belt 11 in a reciprocating spraying manner to form a thin-layer material, and the thickness of the material is 8 mm.
[0128] Under the action of the vacuum component 18, a vacuum environment is formed inside the steam generation device. As the conveyor belt 11 moves, the material moves above the first temperature control component 13, and the material on the conveyor belt 11 is heated under vacuum conditions through the contact between the conveyor belt 11 and the first temperature control component 13 to generate vapor containing 1,5-pentanediamine; under the action of the vacuum component 18, the vapor containing 1,5-pentanediamine is discharged from the steam generation device and enters the condensation device 30, and is condensed into a liquid under the action of the condensation device 30.
[0129] Pass the condensed liquid into a distillation column for rectification treatment to obtain 1,5-pentanediamine product. The test results of the purity, color number, and tetrahydropyridine content of the obtained 1,5-pentanediamine product are shown in Table 1. Among them, the bottom temperature of the distillation column is 120 °C, the top temperature of the distillation column is 45 °C, the tower pressure is -0.09 MPa, the number of theoretical plates is 40, and the top reflux ratio is 2.
[0130] In addition, as the conveyor belt 11 moves, the remaining residue on the conveyor belt 11 moves above the second temperature control component 14, and the material on the conveyor belt 11 is subjected to a second heating treatment at 110 °C through the contact between the conveyor belt 11 and the second temperature control component 14. After the second heating treatment, the residue moves to the winding end along with the conveyor belt 11. The large pieces of material are broken by the reciprocating breaking component 15 and fall into the storage tank, and then are transported out of the steam generation device to obtain solid particles. The test results of the residual amount of 1,5-pentanediamine in the solid particles are shown in Table 1.
[0131] Among them, the heating method of the first temperature control component 13 is heating with heat transfer oil, the heating temperature is 215 °C, and the vacuum degree in the steam generation device is 400 Pa (absolute pressure). The residence time of the material above the first temperature control component 13 is 90 min.
[0132] Example 2
[0133] Preheat the alkalized solution containing 1,5-pentanediamine in the feed tank 40 (the solid content of the alkalized solution is 50%, the mass concentration of 1,5-pentanediamine in the alkalized solution is 22%, the density of the alkalized solution is 1.20, the pH of the alkalized solution is 12.8, and the proportion of alkali metal salts in the solid matter of the alkalized solution is 50%) to 90 °C; pass the preheated raw material liquid into the cloth-feeding component 10 through the feed pump 50, and continuously spread the raw material liquid on the conveyor belt 11 in a reciprocating spraying manner to form a thin-layer material, and the thickness of the material is 8 mm.
[0134] Under the action of the vacuum component 18, a vacuum environment is formed inside the steam generation device. As the conveyor belt 11 moves, the material moves above the first temperature control component 13, and the material on the conveyor belt 11 is heated under vacuum conditions through the contact between the conveyor belt 11 and the first temperature control component 13 to generate vapor containing 1,5-pentanediamine; under the action of the vacuum component 18, the vapor containing 1,5-pentanediamine is discharged from the steam generation device and enters the condensation device 30, and is condensed into a liquid under the action of the condensation device 30.
[0135] Pass the condensed liquid into a distillation column for distillation treatment to obtain 1,5-pentanediamine products. The test results of the purity, color number, and tetrahydropyridine content of the obtained 1,5-pentanediamine products are shown in Table 1. Among them, the bottom temperature of the distillation column is 120 °C, the top temperature of the distillation column is 45 °C, the column pressure is -0.09 MPa, the number of theoretical plates is 40, and the top reflux ratio is 2.
[0136] In addition, as the conveyor belt 11 moves, the remaining residue on the conveyor belt 11 moves above the second temperature control component 14, and the material on the conveyor belt 11 is subjected to a second heating treatment at 90 °C through the contact between the conveyor belt 11 and the second temperature control component 14. After the second heating treatment, the residue moves to the winding end along with the conveyor belt 11. The large pieces of material are broken by the reciprocating breaking component 15 and fall into the storage tank, and then are transported out of the steam generation device to obtain solid particles. The test results of the residual amount of 1,5-pentanediamine in the solid particles are shown in Table 1.
[0137] Among them, the heating method of the first temperature control component 13 is heat-conducting oil heating, the heating temperature is 215 °C, and the vacuum degree in the steam generation device is 1500 Pa (absolute pressure). The residence time of the material above the first temperature control component 13 is 90 min.
[0138] Example 3
[0139] Preheat the alkalized solution containing 1,5-pentanediamine in the feed tank 40 (the solid content of the alkalized solution is 15%, the mass concentration of 1,5-pentanediamine in the alkalized solution is 60%, the density of the alkalized solution is 1.16, the pH of the alkalized solution is 12.8, and the proportion of alkali metal salts in the solid matter of the alkalized solution is 50%) to 95 °C; pass the preheated raw material liquid into the cloth component 10 through the feed pump 50, and continuously spread the raw material liquid on the conveyor belt 11 in a reciprocating spraying manner to form a thin-layer material, and the thickness of the material is 8 mm.
[0140] Under the action of the vacuum component 18, a vacuum environment is formed inside the steam generation device. As the conveyor belt 11 moves, the material moves above the first temperature control component 13, and the material on the conveyor belt 11 is heated under vacuum conditions through the contact between the conveyor belt 11 and the first temperature control component 13 to generate vapor containing 1,5-pentanediamine; under the action of the vacuum component 18, the vapor containing 1,5-pentanediamine is discharged from the steam generation device and enters the condensation device 30, and is condensed into a liquid under the action of the condensation device 30.
[0141] Pass the condensed liquid into a distillation column for rectification treatment to obtain a 1,5-pentanediamine product. The test results of the purity, color number, and tetrahydropyridine content of the obtained 1,5-pentanediamine product are shown in Table 1. Among them, the bottom temperature of the rectification column is 120 °C, the top temperature of the rectification column is 45 °C, the column pressure is -0.09 MPa, the number of theoretical plates is 40, and the top reflux ratio is 2.
[0142] In addition, as the conveyor belt 11 moves, the remaining residue on the conveyor belt 11 moves above the second temperature control component 14, and the material on the conveyor belt 11 is subjected to a second heating treatment at 105 °C through the contact between the conveyor belt 11 and the second temperature control component 14. After the second heating treatment, the residue moves to the winding end along with the conveyor belt 11. The large pieces of material are broken by the reciprocating crushing component 15 and fall into the storage tank, and then are transported out of the steam generation device to obtain solid particles. The test results of the residual amount of 1,5-pentanediamine in the solid particles are shown in Table 1.
[0143] Among them, the heating method of the first temperature control component 13 is heat-conducting oil heating, the heating temperature is 215 °C, and the vacuum degree in the steam generation device is 400 Pa (absolute pressure). The residence time of the material above the first temperature control component 13 is 90 min.
[0144] Example 4
[0145] The alkalized solution containing 1,5-pentanediamine in the feed tank 40 (the solid content of the alkalized solution is 35%, the mass concentration of 1,5-pentanediamine in the alkalized solution is 60%, the density of the alkalized solution is 1.17, the pH of the alkalized solution is 12.6, and the proportion of alkali metal salts in the solid matter of the alkalized solution is 35%) is preheated to 98 °C; the preheated raw material solution is passed into the cloth spreading component 10 through the feed pump 50, and the raw material solution is continuously spread on the conveyor belt 11 in a reciprocating spraying manner to form a thin-layer material, and the thickness of the material is 8 mm.
[0146] Under the action of the vacuum component 18, a vacuum environment is formed inside the steam generation device. As the conveyor belt 11 moves, the material moves above the first temperature control component 13, and the material on the conveyor belt 11 is heated under vacuum conditions through the contact between the conveyor belt 11 and the first temperature control component 13 to generate vapor containing 1,5-pentanediamine; under the action of the vacuum component 18, the vapor containing 1,5-pentanediamine is discharged from the steam generation device and enters the condensation device 30, and is condensed into a liquid under the action of the condensation device 30.
[0147] The condensed liquid is passed into a distillation column for rectification treatment to obtain a 1,5-pentanediamine product. The test results of the purity, color number, and tetrahydropyridine content of the obtained 1,5-pentanediamine product are shown in Table 1. Among them, the bottom temperature of the distillation column is 120 °C, the top temperature of the distillation column is 45 °C, the column pressure is -0.09 MPa, the number of theoretical plates is 40, and the top reflux ratio is 2.
[0148] In addition, as the conveyor belt 11 moves, the remaining residue on the conveyor belt 11 moves above the second temperature control component 14, and the material on the conveyor belt 11 is subjected to a second heating treatment at 112 °C through the contact between the conveyor belt 11 and the second temperature control component 14. After the second heating treatment, the residue moves to the winding end along with the conveyor belt 11. The large pieces of material are broken by the reciprocating breaking component 15 and fall into the storage tank, and then are transported out of the steam generation device to obtain solid particles. The test results of the residual amount of 1,5-pentanediamine in the solid particles are shown in Table 1.
[0149] Among them, the heating method of the first temperature control component 13 is heat-conducting oil heating, the heating temperature is 215 °C, and the vacuum degree inside the steam generation device is 400 Pa (absolute pressure). The residence time of the material above the first temperature control component 13 is 90 min.
[0150] Example 5
[0151] Preheat the alkalized solution containing 1,5-pentanediamine in the feed tank 40 (the solid content of the alkalized solution is 35%, the mass concentration of 1,5-pentanediamine in the alkalized solution is 60%, the density of the alkalized solution is 1.18, the pH of the alkalized solution is 12.6, and the proportion of alkali metal salts in the solid matter of the alkalized solution is 70%) to 100 °C; pass the preheated raw material liquid into the cloth-feeding component 10 through the feed pump 50, and continuously spread the raw material liquid on the conveyor belt 11 in a reciprocating spraying manner to form a thin-layer material, and the thickness of the material is 8 mm.
[0152] Under the action of the vacuum component 18, a vacuum environment is formed inside the steam generation device. As the conveyor belt 11 moves, the material moves above the first temperature control component 13, and the material on the conveyor belt 11 is heated under vacuum conditions through the contact between the conveyor belt 11 and the first temperature control component 13 to generate vapor containing 1,5-pentanediamine; under the action of the vacuum component 18, the vapor containing 1,5-pentanediamine is discharged from the steam generation device and enters the condensation device 30, and is condensed into a liquid under the action of the condensation device 30.
[0153] Pass the condensed liquid into a distillation column for rectification treatment to obtain 1,5-pentanediamine product. The test results of the purity, color number, and tetrahydropyridine content of the obtained 1,5-pentanediamine product are shown in Table 1. Among them, the bottom temperature of the distillation column is 120 °C, the top temperature of the distillation column is 45 °C, the column pressure is -0.09 MPa, the number of theoretical plates is 40, and the top reflux ratio is 2.
[0154] In addition, as the conveyor belt 11 moves, the remaining residue on the conveyor belt 11 moves above the second temperature control component 14, and the material on the conveyor belt 11 is subjected to a second heating treatment at 110 °C through the contact between the conveyor belt 11 and the second temperature control component 14. After the second heating treatment, the residue moves to the winding end along with the conveyor belt 11. The large pieces of material are broken by the reciprocating crushing component 15 and fall into the storage tank, and then are transported out of the steam generation device to obtain solid particles. The test results of the residual amount of 1,5-pentanediamine in the solid particles are shown in Table 1.
[0155] Among them, the heating method of the first temperature control component 13 is heat-conducting oil heating, the heating temperature is 215 °C, and the vacuum degree in the steam generation device is 400 Pa (absolute pressure). The residence time of the material above the first temperature control component 13 is 90 min.
[0156] Example 6
[0157] The alkalized solution containing 1,5-pentanediamine in the feed tank 40 (the solid content of the alkalized solution is 35%, the mass concentration of 1,5-pentanediamine in the alkalized solution is 60%, the density of the alkalized solution is 1.18, the pH of the alkalized solution is 12.8, and the proportion of alkali metal salts in the solid matter of the alkalized solution is 50%) is preheated to 98°C; the preheated raw material liquid is passed into the cloth spreading component 10 through the feed pump 50, and the raw material liquid is continuously spread on the conveyor belt 11 in a reciprocating spraying manner to form a thin-layer material, and the thickness of the material is 4 mm.
[0158] Under the action of the vacuum component 18, a vacuum environment is formed inside the steam generation device. As the conveyor belt 11 moves, the material moves above the first temperature control component 13, and the material on the conveyor belt 11 is heated under vacuum conditions through the contact between the conveyor belt 11 and the first temperature control component 13 to generate vapor containing 1,5-pentanediamine; under the action of the vacuum component 18, the vapor containing 1,5-pentanediamine is discharged from the steam generation device and enters the condensation device 30, and is condensed into a liquid under the action of the condensation device 30.
[0159] The condensed liquid is passed into a distillation column for rectification treatment to obtain 1,5-pentanediamine products. The test results of the purity, color number, and tetrahydropyridine content of the obtained 1,5-pentanediamine products are shown in Table 1. Among them, the bottom temperature of the rectification column is 120°C, the top temperature of the rectification column is 45°C, the column pressure is -0.09 MPa, the number of theoretical plates is 40, and the top reflux ratio is 2.
[0160] In addition, as the conveyor belt 11 moves, the remaining residue on the conveyor belt 11 moves above the second temperature control component 14, and the material on the conveyor belt 11 is subjected to a second heating treatment at 110°C through the contact between the conveyor belt 11 and the second temperature control component 14. After the second heating treatment, the residue moves to the winding end with the conveyor belt 11. The large-piece material is broken by the reciprocating crushing component 15 and falls into the storage tank, and then is transported out of the steam generation device to obtain solid particles. The test results of the residual amount of 1,5-pentanediamine in the solid particles are shown in Table 1.
[0161] Among them, the heating method of the first temperature control component 13 is heat-conducting oil heating, the heating temperature is 215°C, and the vacuum degree in the steam generation device is 400 Pa (absolute pressure). The residence time of the material above the first temperature control component 13 is 55 min.
[0162] Example 7
[0163] Preheat the alkalized solution containing 1,5-pentanediamine in the feed tank 40 (the solid content of the alkalized solution is 35%, the mass concentration of 1,5-pentanediamine in the alkalized solution is 60%, the density of the alkalized solution is 1.18, the pH of the alkalized solution is 12.8, and the proportion of alkali metal salts in the solid matter of the alkalized solution is 50%) to 100 °C; pass the preheated raw material liquid into the cloth-feeding component 10 through the feed pump 50, and continuously spread the raw material liquid on the conveyor belt 11 in a reciprocating spraying manner to form a thin-layer material, and the thickness of the material is 28 mm.
[0164] Under the action of the vacuum component 18, a vacuum environment is formed inside the steam generation device. As the conveyor belt 11 moves, the material moves above the first temperature control component 13, and the material on the conveyor belt 11 is heated under vacuum conditions through the contact between the conveyor belt 11 and the first temperature control component 13 to generate vapor containing 1,5-pentanediamine; under the action of the vacuum component 18, the vapor containing 1,5-pentanediamine is discharged from the steam generation device and enters the condensation device 30, and is condensed into a liquid under the action of the condensation device 30.
[0165] Pass the condensed liquid into a distillation column for rectification treatment to obtain a 1,5-pentanediamine product. The test results of the purity, color number, and tetrahydropyridine content of the obtained 1,5-pentanediamine product are shown in Table 1. Among them, the bottom temperature of the distillation column is 120 °C, the top temperature of the distillation column is 45 °C, the column pressure is -0.09 MPa, the number of theoretical plates is 40, and the top reflux ratio is 2.
[0166] In addition, as the conveyor belt 11 moves, the remaining residue on the conveyor belt 11 moves above the second temperature control component 14, and the material on the conveyor belt 11 is subjected to a second heating treatment at 110 °C through the contact between the conveyor belt 11 and the second temperature control component 14. After the second heating treatment, the residue moves to the winding end along with the conveyor belt 11. The large pieces of material are broken by the reciprocating breaking component 15 and fall into the storage tank, and then are transported out of the steam generation device to obtain solid particles. The test results of the residual amount of 1,5-pentanediamine in the solid particles are shown in Table 1.
[0167] Among them, the heating method of the first temperature control component 13 is heat-conducting oil heating, the heating temperature is 215 °C, and the vacuum degree inside the steam generation device is 400 Pa (absolute pressure). The residence time of the material above the first temperature control component 13 is 90 min.
[0168] Example 8
[0169] Preheat the alkalized solution containing 1,5-pentanediamine in the feed tank 40 (the solid content of the alkalized solution is 35%, the mass concentration of 1,5-pentanediamine in the alkalized solution is 60%, the density of the alkalized solution is 1.18, the pH of the alkalized solution is 12.8, and the proportion of alkali metal salts in the solid matter of the alkalized solution is 50%) to 100 °C; pass the preheated raw material liquid into the cloth component 10 through the feed pump 50, and continuously spread the raw material liquid on the conveyor belt 11 in a reciprocating spraying manner to form a thin-layer material, and the thickness of the material is 8 mm.
[0170] Under the action of the vacuum component 18, a vacuum environment is formed inside the steam generation device. As the conveyor belt 11 moves, the material moves above the first temperature control component 13, and the material on the conveyor belt 11 is heated under vacuum conditions through the contact between the conveyor belt 11 and the first temperature control component 13 to generate vapor containing 1,5-pentanediamine; under the action of the vacuum component 18, the vapor containing 1,5-pentanediamine is discharged from the steam generation device and enters the condensation device 30, and is condensed into a liquid under the action of the condensation device 30.
[0171] Pass the condensed liquid into a distillation column for rectification treatment to obtain a 1,5-pentanediamine product. The test results of the purity, color number, and tetrahydropyridine content of the obtained 1,5-pentanediamine product are shown in Table 1. Among them, the bottom temperature of the distillation column is 120 °C, the top temperature of the distillation column is 45 °C, the column pressure is -0.09 MPa, the number of theoretical plates is 40, and the top reflux ratio is 2.
[0172] In addition, as the conveyor belt 11 moves, the remaining residue on the conveyor belt 11 moves above the second temperature control component 14, and the material on the conveyor belt 11 is subjected to a second heating treatment at 110 °C through the contact between the conveyor belt 11 and the second temperature control component 14. After the second heating treatment, the residue moves to the winding end along with the conveyor belt 11. The large pieces of material are broken by the reciprocating crushing component 15 and fall into the storage tank, and then are transported out of the steam generation device to obtain solid particles. The test results of the residual amount of 1,5-pentanediamine in the solid particles are shown in Table 1.
[0173] Among them, the heating method of the first temperature control component 13 is heat-conducting oil heating, the heating temperature is 235 °C, and the vacuum degree in the steam generation device is 100 Pa (absolute pressure). The residence time of the material above the first temperature control component 13 is 90 min.
[0174] Example 9
[0175] Preheat the alkalized liquid containing 1,5-pentanediamine in the feed tank 40 (the solid content of the alkalized liquid is 35%, the mass concentration of 1,5-pentanediamine in the alkalized liquid is 60%, the density of the alkalized liquid is 1.18, the pH of the alkalized liquid is 12.8, and the proportion of alkali metal salts in the solid matter of the alkalized liquid is 50%) to 100 °C; pass the preheated raw material liquid into the cloth component 10 through the feed pump 50, and continuously spread the raw material liquid on the conveyor belt 11 in a reciprocating spraying manner to form a thin-layer material, and the thickness of the material is 8 mm.
[0176] Under the action of the vacuum component 18, a vacuum environment is formed inside the steam generating device. As the conveyor belt 11 moves, the material moves above the first temperature control component 13, and the material on the conveyor belt 11 is heated under vacuum conditions through the contact between the conveyor belt 11 and the first temperature control component 13 to generate vapor containing 1,5-pentanediamine; under the action of the vacuum component 18, the vapor containing 1,5-pentanediamine is discharged from the steam generating device and enters the condensation device 30, and is condensed into a liquid under the action of the condensation device 30.
[0177] Pass the condensed liquid into a distillation column for rectification treatment to obtain a 1,5-pentanediamine product. The test results of the purity, color number, and tetrahydropyridine content of the obtained 1,5-pentanediamine product are shown in Table 1. Among them, the bottom temperature of the distillation column is 120 °C, the top temperature of the distillation column is 45 °C, the column pressure is -0.09 MPa, the number of theoretical plates is 40, and the top reflux ratio is 2.
[0178] In addition, as the conveyor belt 11 moves, the remaining residue on the conveyor belt 11 moves above the second temperature control component 14, and the material on the conveyor belt 11 is subjected to a second heating treatment at 110 °C through the contact between the conveyor belt 11 and the second temperature control component 14. After the second heating treatment, the residue moves to the winding end along with the conveyor belt 11. The large pieces of material are broken by the reciprocating breaking component 15 and fall into the storage tank, and then are transported out of the steam generating device to obtain solid particles. The test results of the residual amount of 1,5-pentanediamine in the solid particles are shown in Table 1.
[0179] Among them, the heating method of the first temperature control component 13 is heat-conducting oil heating, the heating temperature is 150 °C, and the vacuum degree in the steam generating device is 6000 Pa (absolute pressure). The residence time of the material above the first temperature control component 13 is 90 min.
[0180] Example 10
[0181] The alkalized solution containing 1,5-pentanediamine in the feed tank 40 (the solid content of the alkalized solution is 35%, the mass concentration of 1,5-pentanediamine in the alkalized solution is 60%, the density of the alkalized solution is 1.18, the pH of the alkalized solution is 12.8, and the proportion of alkali metal salts in the solid matter in the alkalized solution is 50%) is preheated to 96 °C; the preheated raw material liquid is passed into the cloth spreading component 10 through the feed pump 50, and the raw material liquid is continuously spread on the conveyor belt 11 in a reciprocating spraying manner to form a thin-layer material, and the thickness of the material is 8 mm.
[0182] Under the action of the vacuum component 18, a vacuum environment is formed inside the steam generation device. As the conveyor belt 11 moves, the material moves to the upper part of the first temperature control component 13, and the material on the conveyor belt 11 is heated under vacuum conditions through the contact between the conveyor belt 11 and the first temperature control component 13 to generate vapor containing 1,5-pentanediamine; under the action of the vacuum component 18, the vapor containing 1,5-pentanediamine is discharged from the steam generation device and enters the condensation device 30, and is condensed into a liquid under the action of the condensation device 30.
[0183] The condensed liquid is passed into a distillation column for rectification treatment to obtain 1,5-pentanediamine product. The test results of the purity, color number, and tetrahydropyridine content of the obtained 1,5-pentanediamine product are shown in Table 1. Among them, the bottom temperature of the rectification column is 120 °C, the top temperature of the rectification column is 45 °C, the column pressure is -0.09 MPa, the number of theoretical plates is 40, and the top reflux ratio is 2.
[0184] In addition, as the conveyor belt 11 moves, the remaining residue on the conveyor belt 11 moves to the upper part of the second temperature control component 14, and the material on the conveyor belt 11 is subjected to a second heating treatment at 110 °C through the contact between the conveyor belt 11 and the second temperature control component 14. After the second heating treatment, the residue moves to the winding end along with the conveyor belt 11. The large pieces of material are broken by the reciprocating breaking component 15 and fall into the storage tank, and then are transported out of the steam generation device to obtain solid particles. The test results of the residual amount of 1,5-pentanediamine in the solid particles are shown in Table 1.
[0185] Among them, the heating method of the first temperature control component 13 is heat-conducting oil heating, the heating temperature is 215 °C, and the vacuum degree in the steam generation device is 400 Pa (absolute pressure). The residence time of the material above the first temperature control component 13 is 240 min.
[0186] Example 11
[0187] Preheat the alkalized solution containing 1,5-pentanediamine in the feed tank 40 (the solid content of the alkalized solution is 35%, the mass concentration of 1,5-pentanediamine in the alkalized solution is 60%, the density of the alkalized solution is 1.18, the pH of the alkalized solution is 12.8, and the proportion of alkali metal salts in the solid matter of the alkalized solution is 50%) to 100 °C; pass the preheated raw material liquid into the cloth-feeding component 10 through the feed pump 50, and continuously spread the raw material liquid on the conveyor belt 11 in a reciprocating spraying manner to form a thin-layer material, and the thickness of the material is 8 mm.
[0188] Under the action of the vacuum component 18, a vacuum environment is formed inside the steam generation device. As the conveyor belt 11 moves, the material moves above the first temperature control component 13, and the material on the conveyor belt 11 is heated under vacuum conditions through the contact between the conveyor belt 11 and the first temperature control component 13 to generate vapor containing 1,5-pentanediamine; under the action of the vacuum component 18, the vapor containing 1,5-pentanediamine is discharged from the steam generation device and enters the condensation device 30, and is condensed into a liquid under the action of the condensation device 30.
[0189] Pass the condensed liquid into a distillation column for rectification treatment to obtain a 1,5-pentanediamine product. The test results of the purity, color number, and tetrahydropyridine content of the obtained 1,5-pentanediamine product are shown in Table 1. Among them, the bottom temperature of the distillation column is 120 °C, the top temperature of the distillation column is 45 °C, the column pressure is -0.09 MPa, the number of theoretical plates is 40, and the top reflux ratio is 2.
[0190] In addition, as the conveyor belt 11 moves, the remaining residue on the conveyor belt 11 moves above the second temperature control component 14, and the material on the conveyor belt 11 is subjected to a second heating treatment at 110 °C through the contact between the conveyor belt 11 and the second temperature control component 14. After the second heating treatment, the residue moves to the winding end with the conveyor belt 11. The large pieces of material are broken by the reciprocating breaking component 15 and fall into the conveying trough with a crushing function. The residue is crushed in the conveying trough and then conveyed out of the steam generation device to obtain solid particles. The test results of the residual amount of 1,5-pentanediamine in the solid particles are shown in Table 1.
[0191] Among them, the heating method of the first temperature control component 13 is heating with heat-conducting oil, the heating temperature is 215 °C, and the vacuum degree in the steam generation device is 400 Pa (absolute pressure). The residence time of the material above the first temperature control component 13 is 25 min.
[0192] Table 1 Test result table of product indicators
[0193]
[0194] Unless otherwise specified, the terms used in the present invention have the meanings commonly understood by those skilled in the art.
[0195] The embodiments described in the present invention are for illustrative purposes only and are not intended to limit the scope of protection of the present invention. Those skilled in the art can make various other substitutions, changes, and improvements within the scope of the present invention. Therefore, the present invention is not limited to the above embodiments but is only defined by the claims.
Claims
1. A system for separating 1,5-pentanediamine, comprising: A vapor generation device for heating a raw material solution containing 1,5-pentanediamine to obtain a vapor containing 1,5-pentanediamine; And A refining device for refining the liquid obtained after condensing the vapor containing 1,5-pentanediamine to obtain 1,5-pentanediamine; Wherein, the vapor generation device includes a conveyor belt, a driving component and a temperature control component; the conveyor belt is used to carry the raw material solution, the temperature control component is used to heat the raw material solution on the conveyor belt, and the driving component is used to drive the conveyor belt to rotate in a cycle; The vapor generation device includes a cloth component for arranging the raw material solution containing 1,5-pentanediamine on the conveyor belt; The vapor generation device includes a vacuum component.
2. The system for separating 1,5-pentanediamine according to claim 1, wherein, The refining device includes one or more of a rectification device, a distillation device, and an evaporation device; And / or, the temperature control component includes a first temperature control component, and the first temperature control component is used to perform a first heating treatment on the raw material solution containing 1,5-pentanediamine to form the vapor containing 1,5-pentanediamine and a residue-containing remainder.
3. The system for separating 1,5-pentanediamine according to claim 2, wherein, The driving component includes a first roller and a second roller, and the conveyor belt is sleeved on the first roller and the second roller; along the transmission direction of the conveyor belt, the temperature control component is located between the first roller and the second roller; and / or, The temperature control component includes a second temperature control component, and the second temperature control component is used to perform a second heating treatment on the residue-containing remainder.
4. The system for separating 1,5-pentanediamine according to claim 3, wherein The vapor generation device includes a crushing component for crushing the residue, and the crushing component is arranged outside the second roller.
5. The system for separating 1,5-pentanediamine according to claim 1, wherein, The vapor generation device includes a housing having an accommodation space, the conveyor belt, the driving component, and the temperature control component are located in the accommodation space of the housing, and a heat insulation layer is provided on the housing.
6. The system for separating 1,5-pentanediamine according to claim 1, comprising a condensation device, and the condensation device is respectively connected to the vapor generation device and the refining device.
7. The system for separating 1,5-pentanediamine according to claim 1, comprising a feed tank, the feed tank includes a stirring component and / or a third temperature control component, and the feed tank is connected to the vapor generation device through a feed pump.
8. The system for separating 1,5-pentanediamine according to claim 7, comprising a concentration tank, and the feed tank is respectively connected to the concentration tank and the vapor generation device.
9. A method for separating 1,5-pentanediamine, comprising: Heating a raw material solution containing 1,5-pentanediamine through a vapor generation device to obtain a vapor containing 1,5-pentanediamine; And Refining the liquid obtained after condensing the vapor containing 1,5-pentanediamine to obtain a 1,5-pentanediamine product; Among them, the vapor generation device includes a conveyor belt, a driving component, and a temperature control component; the conveyor belt is used to carry the raw material liquid, the temperature control component is used to heat-treat the raw material liquid on the conveyor belt, and the driving component is used to drive the conveyor belt to rotate in a cycle.
10. The method according to claim 9, wherein, By adding an alkaline substance to a solution system containing 1,5-pentanediamine salt, the 1,5-pentanediamine salt therein reacts with the alkaline substance to obtain the raw material liquid containing 1,5-pentanediamine. The solution system containing 1,5-pentanediamine salt includes a fermentation broth or an enzyme conversion broth containing 1,5-pentanediamine salt.
11. The method according to claim 9, wherein, The solid content of the raw material liquid containing 1,5-pentanediamine is 10-80%; and / or The raw material liquid containing 1,5-pentanediamine contains an alkali metal salt, and the mass of the alkali metal salt accounts for 30-80% of the mass of the solids in the raw material liquid containing 1,5-pentanediamine; and / or The mass content of 1,5-pentanediamine in the raw material liquid containing 1,5-pentanediamine is 8%-75%; and / or The pH of the raw material liquid containing 1,5-pentanediamine > 12.3; and / or The density of the raw material liquid containing 1,5-pentanediamine is 1.02 to 1.25 g / cm 3 ; and / or, The feeding temperature of the raw material liquid containing 1,5-pentanediamine into the vapor generation device is 40-130°C.
12. The method according to claim 9, wherein, The heat treatment includes a first heat treatment. After the raw material liquid containing 1,5-pentanediamine undergoes the first heat treatment, it forms vapor containing 1,5-pentanediamine and a residue-containing remainder.
13. The method according to claim 12, wherein, The time for the raw material liquid containing 1,5-pentanediamine to undergo the first heat treatment is 20-300 min; and / or The temperature of the first heat treatment is 105-250°C, and the vacuum degree is 10 Pa-10 kPa.
14. The method according to claim 12, wherein, It further includes subjecting the residue-containing remainder to a second heat treatment, and the temperature of the second heat treatment is 50-180°C.
15. The method according to claim 9 includes condensing the vapor containing 1,5-pentanediamine into a liquid and then performing the refining treatment.
16. The method according to claim 9 or 15, wherein the refining treatment comprises: One or more of rectification, distillation, evaporation.
17. The method according to claim 9, wherein, The vapor generation device is a belt dryer.
18. The method according to claim 17, wherein, The belt dryer is a vacuum belt dryer.
Citation Information
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